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no


Analytical Abstracts

; reprint available!

Record 1 of 57 ;

TI: Analysis of toxic wastes in tissues from aquatic species. Applications of matrix solid-phase
dispersion.
AU: Crouch,-MD; Barker,-SA
AD: Louisiana State Univ., Lab. Residue Studies, School Vet. Med., Baton Rouge, LA 70803, USA
SO: J-Chromatogr,-A. 11 Jul 1997; 774(1-2): 287-309
AB: A review is presented that surveys problems of extraction of toxic waste components (such as
PAH, PCB, organochlorine compounds and pesticides) from aquatic biological matrices (such as
tissues from fish, shellfish and amphibians), including regulatory legislation. Toxic contaminants
typically present in various biological species matrices are tabulated. The matrix solid-phase
dispersion analysis of toxic agricultural compounds in four matrices and of PAH and PCB in one
matrix (catfish muscle) is examined. Subsequent analyses of extracts are by GC or HPLC. Present
developments in the field are described and future ones discussed. (175 references).
Record 2 of 57

TI: Veterinary drug residues survey in meat: an HPLC method with a matrix solid-phase dispersion
extraction.
AU: Le-Boulaire,-S; Bauduret,-J-C; Andre,-F
AD: Nestle France, Lab. Contole, 95806 Cergy Pontoise, France
SO: J-Agric-Food-Chem. Jun 1997; 45(6): 2134-2142
AB: Meat was extracted using matrix solid-phase dispersion with C18. Two fractions were eluted
with CH2Cl2 and ethyl acetate which were dried at 40degreeC. The respective residues were
reconstituted with 0.01M-ammonium acetate buffer of pH 5.2/acetonitrile/methanol (43:5:2 and
56:31:13). HPLC was performed on a 5 micro m Spherisorb C18 ODS II column (25 cm x 4.6 mm
i.d.) operated at 35degreeC with gradient elution (1 or 0.5 ml/min) with 0.01M-ammonium acetate
buffer of pH 5.2/acetonitrile/methanol (details given for each fraction) and diode-array detection at
270 and 365 nm for the first fraction and 254, 291 and 348 nm for the second fraction. The second
fraction was also detected by fluorescence at 365 nm (excitation at 308 nm). Calibration graphs
were linear from 50-250 ppb and detection limits were The method was used to determine 14
veterinary drug residues in meat.
Record 3 of 57

TI: Fluorodensitometric residue analysis of sulphaguanidine and sulphadimidine after MSPD-clean
up of aluminium oxide.
AU: Glaser,-B; Petz,-M
AD: Bergische Univ. GH Wuppertal, Wuppertal, Germany
SO: Lebensmittelchemie. 1996; 50(1): 9
AB: The use of C18 cartridges for the isolation of the sulphonamide drugs from animal samples
gave poor recoveries because of irreversible adsorption. Subsequent HPLC determination also
caused problems because of early elution, especially of sulphaguanidine. These problems were
overcome by the use of the aluminium oxide matrix solid-phase dispersion (MSPD) technique of
Barker etal. (J. Chromatogr., 1989, 475, 353). The sulphonamide drugs were eluted from the
aluminium oxide with a mixture of acetonitrile and saturated Na2CO3 solution and were separated
by TLC. The spots were located by dipping the plate in fluorescamine solution, with densitometric
measurement of the fluorescence. This procedure gave 70-90% recovery of 50-200 ppb of the
three sulphonamides from tissues and fluids without matrix interference.
Record 4 of 57

TI: Optimization of matrix solid-phase dispersion method for the analysis of pesticide residues in
vegetables.
AU: Viana,-E; Molto,-JC; Font,-G
AD: Univ. Valencia, Lab. Food Chem. and Toxicol., Fac. Pharm., 46100 Burjassot, Valencia, Spain
SO: J-Chromatogr,-A. 22 Nov 1996; 754(1-2): 437-444
AB: A multiresidue method based on matrix solid-phase dispersion was developed for extracting
chlorfenvinfos, chlorpyrifos, fenarimol, iprodione, procimydone, propiconazole, tetradifon,
triadimefon and vinclozolin from artichokes, green beans, lettuce and tomato. A mixture of 5 g
chopped vegetables, 10 g Florisil (60-100 mesh) and 8 g acid washed sand was ground to a
homogeneous flowing powder. The powder was transferred to an extraction column (40 cm x 3 cm
i.d.) with 2 x 50 ml CH2Cl2. The CH2Cl2 extract was collected and reduced to 10 ml by
evaporation at 60degreeC and the solvent was changed to 1 ml methanol. The extract was purified
by SPE using octyl-silica Bondapak (37-55 micro m) and 5 ml ethyl acetate as eluent. The eluate
was reduced to 1 ml and a 2 micro l portion was analysed by GC-ECD on a column (30 m x 0.25
mm i.d.) coated with DB-5 (0.25 micro m) with He as carrier gas (2.8 ml/min) and temperature
programming from 50degreeC (held for 0.8 min) to 140degreeC (held for 2 min) at 30degreeC/min
and then to 280degreeC (held for 12 min) at 5degreeC/min. The mean recovery of the target
pesticides from vegetables spiked at the 18-95 ng/g level was 91% and the RSD were The
method was used to analyse vegetables from local markets.
Record 5 of 57

TI: Determination of pesticide residues in fruit and vegetables.
AU: Torres,-CM; Pico,-Y; Manes,-J
AD: Univ. Valencia, Lab. Bromatol. i Toxicol., Fac. Farm., 46100 Burjassot, Valencia, Spain
SO: J-Chromatogr,-A. 22 Nov 1996; 754(1-2): 301-331
AB: A review is presented on methods based on GC, HPLC, SFC and immunoassay for
determining pesticide residues in fruit and vegetables. Extraction and clean up procedures by
liquid-liquid extraction, matrix solid-phase dispersion and SFE are discussed. (185 references).
Record 6 of 57

TI: Pesticide residue analyses in plant material by chromatographic methods: clean up procedures
and selective detectors.
AU: Tekel,-J; Hatrik,-S
AD: Comenius Univ., Fac. Pharm., 832 32 Bratislava, Slovakia
SO: J-Chromatogr,-A. 22 Nov 1996; 754(1-2): 397-410
AB: A review is presented of GC and LC methods for determining pesticide residues in plant
materials. Extraction and clean up procedures based on adsorption column chromatography, GPC,
SFE, matrix solid-phase dispersion and sweep co-distillation are discussed. (99 references).
Record 7 of 57

TI: Determination of polychlorinated biphenyls and chlorinated pesticides in human body fluids and
tissues.
AU: Bucholski,-KA; Begerow,-J; Winneke,-G; Dunemann,-L
AD: Med. Inst. Umwelthygiene, Dept. Anal. Chem., 40225 Duesseldorf, Germany
SO: J-Chromatogr,-A. 22 Nov 1996; 754(1-2): 479-485
AB: A single-stage clean up preconcentration procedure based on matrix solid-phase dispersion
was employed in determining PCB and chlorinated pesticides in human blood serum, milk, bone
marrow and tissue. Samples of up to 5 ml or 1 g were homogenized with up to 6 g activated Florisil
(0.15-0.25 mm particle size). The resulting powder was transferred to a prepacked column (2.2 cm
i.d.) containing up to 15 g Florisil deactivated with 3% H2O. The column was washed with 60 ml
hexane and 80 ml hexane/CH2Cl2 (4:1). Both eluates were collected, combined and reduced to
0.5 ml for analysis by GC-MS or dual-column GC with ECD. Analysis by GC-MS was performed on
a column (50 m x 0.2 mm i.d.) coated with Ultra 2 (0.33 micro m) coupled directly to a quadrupole
MS operated in the selected-ion monitoring mode. The dual-column GC was equipped with a
column (30 m x 0.32 mm i.d.) coated with DB5-MS (0.25 micro m) and a column (30 m x 0.32 mm
i.d.) coated with DB-1701 (0.25 micro m) operating in parallel and two 63Ni electron-capture
detectors. The detection limits for chlorinated pesticides and PCB congeners were 1.3-4 pg and 1-
23.3 pg, respectively, for GC-MS and 0.4-0.8 pg and 0.3-0.7 pg, respectively, for dual-column GC.
Record 8 of 57

TI: Matrix solid-phase dispersion technique for the determination of moxidectin in bovine tissues.
AU: Alvinerie,-M; Sutra,-JF; Capela,-D; Galtier,-P; Fernandez-Suarez,-A; Horne,-E; O'Keeffe,-M
AD: INRA, Lab. Pharmacol.-Toxicol., 31931 Toulouse, France
SO: Analyst (Cambridge, UK). Oct 1996; 121(10): 1469-1472
AB: Homogenized bovine tissue (muscle, liver) (0.25 g) was blended with 1 g C18 end-capped
sorbent. A column was prepared with the resulting material and was washed with 2 ml hexane.
After drying the column, moxidectin (I) was eluted with 6 ml CH2Cl2/ethyl acetate (3:1) onto an
Alumina-B SPE cartridge attached below the column. The SPE cartridge was dried, washed with 1
ml acetone and dried again, after which I was eluted with 6 ml methanol. The eluate was
evaporated to dryness and the residue was treated with N-methylimidazole and trifluoroacetic
anhydride in acetonitrile (cf. Alvinerie et al., J. Chromatogr. B., 1995, 674, 119). A portion (100
micro l) of the reaction mixture was analysed by HPLC on a 3 micro m Supelcosil column (15 cm x
4.6 mm i.d.), with 0.2% acetic acid/methanol/acetontrile (4:15:31) as mobile phase (1.5 ml/min) and
fluorimetric detection at 447 nm (excitation at 383 nm). The calibration graph was linear for 1
(detection limit) to 100 ng/g of I. The inter-assay RSD (n = 5) was Recoveries of I were >80%.
Record 9 of 57

TI: Preparation of sample solution for determination of acid coal-tar dyes in confectionery by the
matrix solid-phase dispersion method.
AU: Kai,-S; Nikkawa,-T; Takahashi,-A; Koizumi,-A; Hyoudou,-Y; Suzuki,-S; Nakazawa,-H
AD: Kanagawa Prefectural Chigasaki Health Centre, Kanagawa 253, Japan
SO: Shokuhin-Eiseigaku-Zasshi. Jun 1996; 37(3): 146-150
AB: Sample (0.5 g) was treated with 0.7 ml methanolic 0.1M-cetyltrimethylammonium bromide (I)
and blended with 2 g octadecylsilyl (C18)-derivatized silica (50 micro m; C18-Sil) as adsorbent
and dried. The C18-Sil and prepared sample matrix were respectively packed into a small column
for percolation with 10 ml H2O. The food dyes (food colourings; FC) were eluted with 5 ml
methanol through a syringe. For qualitative analysis, the eluate was directly applied on to a Kiesel
Gel 60 plate for TLC with ethyl acetate/methanol/28% ammonia H2O (3:3:1) as mobile phase. For
quantitative analysis, the eluate was diluted 5-fold with mobile phase, centrifuged for 5 min and a
20 micro l portion of the supernatant was analysed by HPLC on a Finepak C-18S column (15 cm x
4.6 mm i.d.) operated at 50degreeC with aqueous 77% methanol, containing 25 mg/ml I, as mobile
phase (1 ml/min) and detection at 254 nm. The method was used for the determination of 12
permitted and 4 non-permitted FC (tabulated) in soft-drink powder, candy, chewing gum and
cookie. By standard-additions method, recoveries were 76.7-102.4%.
Record 10 of 57

TI: Latest analytical methods for the residual pesticides in food.
AU: Obana,-H; Hori,-S
AD: Osaka Prefectural Inst. Public Health, Osaka 537, Japan
SO: Jpn-J-Toxicol-Environ-Health. Feb 1996; 42(1): 1-16
AB: A review is presented of the analysis of pesticides in food at sub-ppm levels. Extraction
techniques of matrix solid phase dispersion and SFE, clean up procedures of miniature size
column and gel permeation chromatography and analysis by GC and GC-MS are described. The
importance of multiresidue analysis is commented on. (52 references).
Record 11 of 57 ;

TI: Matrix solid-phase dispersion extraction procedure for multiresidue pesticide analysis in
oranges.
AU: Torres,-CM; Pico,-Y; Redondo,-MJ; Manes,-J
AD: Valencia Univ., Lab. Toxicol., Fac. Pharm., 46100 Burjassot, Valencia, Spain
SO: J-Chromatogr,-A. 5 Jan 1996; 719(1): 95-103
AB: The optimization of a matrix solid-phase dispersion method for detection of 18 insecticides in
oranges was studied, with subsequent determination by GC. Milled whole orange and C18 silica
(each 0.5 g) plus 0.5 ml insecticide in ethyl acetate (when testing method efficiency) were
homogenized and transferred on to silica (0.5 g) in a glass column (10 cm x 9 mm i.d.) and the
pesticide was eluted with 10 ml ethyl acetate for analysis by GC in a column (30 m x 0.25 mm i.d.)
coated with DB-1 (0.25 micro m) operated with temperature programming from 50degreeC (held
0.8 min) by multistep gradient (details given) to 280degreeC (held for 1 min), with He as carrier gas
(1 ml/min) and ECD. The lower limits of detection ranged from 2 ppb for aldrin to 171 ppb for
captafol. Test recoveries ranged from 48+/-5% for tetradifon to 108+/-5% for chlorpyriphos. Test
recovery for each pesticide is tabulated alongside recoveries obtained by three established liquid-
liquid extraction methods.
Record 12 of 57

TI: Methods for the determination of beta-agonists in biological matrices.
AU: Boyd,-D; O'Keefe,-M; Smyth,-MR
AD: Natl. Food Centre, Dublin 15, Ireland
SO: Analyst (Cambridge, UK). Jan 1996; 121(1): 1R-10R
AB: A review is presented of methods for determining beta-agonists in complex biological samples.
Emphasis is placed on sample purification procedures, e.g., solvent extraction and liquid-liquid
partitioning, SPE, immunoaffinity chromatography and matrix solid-phase dispersion. Detection
techniques for beta-agonists, e.g., HPLC, GC-MS and immunoassays, are also discussed. (115
references).
Record 13 of 57 ;

TI: Analysis of pesticide residues in fruit and vegetables by matrix solid-phase dispersion (MSPD)
and different gas chromatography element-selective detectors.
AU: Torres,-CM; Pico,-Y; Manes,-J
AD: Valencia Univ., Lab. Bromatol. Toxicol., Fac. Pharm., 46100 Burjassot, Valencia, Spain
SO: Chromatographia. Dec 1995; 41(11-12): 685-692
AB: Samples (0.5 g) were chopped and mixed before blending with C18 silica. The homogenate
was applied to a glass column (10 cm x 9 mm i.d.) packed with 1.5 g silica. Ethyl acetate (10 ml)
was added and the effluent (15 ml) was collected and concentrated under N2 to 0.5 ml. Portions
(1-2 micro l) of the extract were analysed by GC with a number of different detection methods viz.,
ECD, N-P detection, flame-photometric detection, (S and P modes) and mass-selective detection
in selected-ion monitoring mode. Three GC systems were used: (i) a DB-5 column (30 m x 0.25
mm i.d.; 0.25 micro m) equipped with an ECD and flame-photometric detector; (ii) a DB-1 column
(30 m x 0.25 mm i.d.) equipped with an ECD and a N-P detector; (iv) a BPX-5 column (25 m x 0.22
mm i.d. 0.25 micro m) equipped with a mass spectrometer. Analysis was performed with
temperature programming from 50degreeC (held for 0.8 min) to 100degreeC (held for 2 min) with
30degreeC/min, then to 180degreeC at 10degreeC/min, and then to 280degreeC (held for 5 min)
at 4degreeC/min. The use of the detectors in parallel was also investigated. Recoveries were 41-
108% with RSD of 2-14% over the concentration range 0.5-10 micro g/l.
Record 14 of 57 ;

TI: Screening procedure for organochlorine and organophosphorus pesticide residues in milk using
matrix solid-phase dispersion (MSPD) extraction and gas-chromatographic determination.
AU: Schenck,-FJ; Wagner,-R
AD: Food and Drug Administration, Baltimore, MD 21201, USA
SO: Food-Addit-Contam. Jul-Aug 1995; 12(4): 535-541
AB: Milk (5 ml) was blended with 2 g preconditioned C18 silica and 1.5 ml acetonitrile in a syringe
barrel. The aqueous phase was removed from the column by vacuum aspiration and the pesticides
were eluted with 20 ml acetonitrile directly onto a Florisil SPE column (2 g) containing a top 3 cm
layer of Na2SO4. The eluates were evaporated to dryness under N2 and the residue was
dissolved in 1 ml petroleum ether (solution A). Portions (3 micro l) were analysed by GC for
organochlorine (OC) pesticides (tabulated) on a capillary column (30 m x 0.53 mm i.d.) coated
with DB-608 (1.5 micro m) operated at 190degreeC with He as carrier gas (20 ml/min) and 63Ni
ECD. Portions (3 micro l) of solution A were also analysed for organophosphorus (OP) pesticides
on a capillary column (30 m x 0.53 mm i.d.) coated with DB-1 (1.5 micro m) operated at
185degreeC with He as carrier gas (10 ml/min) and flame-photometric detection. Recoveries were
76-97.8 and 75-104.5%, respectively, for milk spiked with 2-20 and 10-50 ppb, respectively of OC
and OP pesticides. Results for OC pesticides agreed well with those obtained by the AOAC
International multiresidue method of Sawyer et al. (Official Methods of Analysis of the Association
of Official Analytical Chemists, 1990, 15th edition, Helrich, K. (ed.), 274).
Record 15 of 57 ;

TI: Matrix solid-phase dispersion linked to solid-phase extraction for beta-agonists in liver samples:
an update.
AU: Boyd,-D; O'Keeffe,-M; Smyth,-MR
AD: Natl. Food Centre, Dublin 15, Ireland
SO: Anal-Proc. Aug 1995; 32(8): 301-303
AB: Liver (500 mg) was dissolved in 10 micro l ethanol and the solution was spiked with 2 ng each
of salbutamol (I), clenbuterol (II) and mabuterol (III). The solution was blended with 50 micro m
Isolute C18 and 40 micro m Bondesil C18 solid phases and packed into columns. I, II and III were
eluted with 12 ml methanol. The eluates were centrifuged at 2000 rpm for 10 mins and the
supernatants were evaporated to dryness at 60degreeC under N2. The residues were dissolved in
400 micro l phosphate-gelatin buffer of pH 5, 100 micro l Helix pomatia solution (1:9) was added
and the extracts were incubated at 37degreeC for 2h. On cooling, 500 micro l H2O and 80 micro l
1M-NaOH were added to the incubates and the solutions were applied to a C18 SPE cartridge.
The drugs were eluted with 2 ml methanol, the eluates were evaporated under N2 at 60degreeC
and the residues were dissolved in 500 micro l phosphate-gelatin buffer of pH 7. Portions (0.1 ml)
were analysed by RIA by the method of Boyd et al. (Analyst (Cambridge, UK), 1994, 119, 1467).
Mean recoveries were 79-90, 93-135 and 81-81%, respectively, for I, II and III at 1-2 ng of added
drug. The corresponding RSD (n = 5) were 11.7-26.2, 19.1-25.7 and 8.7-15.9%. Detection limits
were 0.17 and 0.57 ng/g, respectively of each drug on the Bondesil and Isolute C18 columns.
Record 16 of 57

TI: Multiresidue matrix solid-phase dispersion method for the determination of six synthetic
pyrethroids in vegetables followed by gas chromatography with electron-capture detection.
AU: Ling,-Y-C; Huang,-I-P
AD: Natl. Tsing Hua Univ., Dept. Chem., Hsinchu 30043, Taiwan
SO: J-Chromatogr,-A. 24 Mar 1995; 695(1): 75-82
AB: A 5 g portion of chopped vegetable was ground with 8 g of Florisil and applied to a glass
column (30 cm x 15 mm i.d.) of anhydrous Na2SO4 (1 cm) and 0.5 g of Florisil compressed to a
bed depth of 13 cm then covered with Na2SO4 (0.1-0.2 cm). Elution was with 60 ml of
acetone/hexane (1:9). The eluate was concentrated to 2, 100 micro l of tribromobiphenyl was
added (internal standard 3.9 micro g/ml) and the solution was diluted to 1 ml and analysed on a
0.25 micro m DB-5 MS column (30 m x 0.25 mm i.d.) with He as carrier gas at 1 ml/min and with
temperature programming from 60-220degreeC at 30degreeC/min and from 220-300degreeC at
3degreeC/min with detection by 70 eV EIMS using a Shimadzu QP-1000 EX MS system. The
method was suitable for the simultaneous determination of fenpropathrin, cyhalothrin, permethrin,
cypermethrin, fenvalerate and deltamethrin. Recoveries were 92-113% and detection limits were
5.1-91.5 ng/g for the cited insecticides in vegetables. The method is proposed as a relatively rapid
screening technique for pyrethroids in vegetables.
Record 17 of 57

TI: Isolation and quantification of ivermectin in bovine milk by matrix solid phase dispersion
(MSPD) extraction and liquid-chromatographic determination.
AU: Schenck,-FJ
AD: US Food and Drug Administration, Baltimore District Lab., Baltimore, MD 21201, USA
SO: J-Liq-Chromatogr. Jan 1995; 18(2): 349-362
AB: Milk (25 ml) was fortified with 50-400 micro l ng/ml ivermectin (500 ng/ml; I) solution and 200
micro l of 500 ng/ml abamectin solution (internal standard) was added. A 5 ml portion of the
solution was blended with 2 g C18 Bondesil (40 micro m) for 2 min. The aqueous phase was
removed and I was eluted with 10 ml ethyl acetate. The eluate was evaporated to dryness at 2.
The residue was reconstituted in 2 ml 40% ethyl acetate in hexane and the solution was cleaned
up on a Bond-Elut SPE column (500 mg). I residues were eluted from the SPE column with 5 ml of
50% ethyl acetate in methanol. The eluate was evaporated to dryness at The residue was
derivatized with 0.1 ml DMF/acetic anhydride/N-methylimidazole (9:3:2) at 95degreeC for 1 h. The
reaction mixture was diluted with 1 ml CHCl3, loaded on to a SPE column and the I residues were
eluted with 2 ml CHCl3. The eluate was evaporated to dryness at A 50 micro l portion was injected
on to a 5 micro m Econosil C18 (25 cm x 4.6 mm i.d.) column was used with a Brownlee Newguard
RP-18 guard column, with methanol/THF/H2O (17:3:1) as mobile phase (1 ml/min), and
fluorescence detection at 455 nm (excitation at 364 nm). Recoveries of 1-8 ppb I from milk were
81-91.5% and the RSD (n = 7) were 4.6-10.3%.
Record 18 of 57

TI: Multiresidue-matrix solid-phase dispersion method for determining 16 organochlorine pesticides
and polychlorinated biphenyls in fish.
AU: Ling,-Y-C; Huang,-I-P
AD: Natl. Tsing Hua Univ., Dept. Chem., Hsinchu, 30043, Taiwan
SO: Chromatographia. Mar 1995; 40(5-6): 259-266
AB: Fish fillet (0.5 g) was blended with 2 g C18 and the resulting material was placed in a glass
syringe barrel containing 1 g Florisil at the bottom. Elution was effected under gravitational flow
with n-hexane/acetone (9:1) and after the flow ceased the excess eluent was removed from the
column under vacuum. The eluate was concentrated to 2 and 50 micro l dibromo-
octafluorobiphenyl solution in n-hexane (4 ppm; internal standard) was added and the volume was
adjusted to 100 micro l. The eluate was analysed by GC on a column (30 m x 0.25 mm i.d.) coated
with DB-SMS (0.25 micro m) operated with temperature programming from 70degreeC (held for 2
min) to 180degreeC (held for 2 min) at 20degreeC/min, and then to 300degreeC (held for 4 min) at
10degreeC/min, with He as carrier gas (1 ml/min) and 70 eV EIMS detection (m/z tabulated).
Detection limits were 19.6-91.1 ng/g and 71.4-111.2 ng/g for organochlorine pesticides and PCB,
respectively. Recoveries were >85% for all the organochlorine pesticides except heptachlor (78%)
and 4,4'-DDT (81%); recoveries of >95% were obtained for PCB.
Record 19 of 57

TI: Matrix solid-phase dispersion and high-performance liquid-chromatographic determination of
trace isoprocarb and deltamethrin.
AU: Yang,-R; Fu,-CG
AD: Hebei Univ., Res. Centre Phys. and Chem. Anal., Baoding 071002, China
SO: Sepu. Nov 1994; 12(6): 431-432, 435
AB: Food sample (0.5 g) was ground with ODS bonded phase (100-140 mesh) and packed into a
glass syringe. The column was washed with 8 ml cyclohexane, deltamethrin (I) and isoprocarb (II)
were eluted with 6 ml toluene. The eluate was evaporated to dryness, the residue was dissolved in
500 micro l methanol and the solution was centrifuged at 1700 rpm for 10 min. Portions (10 micro l)
of the supernatant were analysed by HPLC on a 5 micro m PE HS-5 C18 column (12.5 cm x 4.6
mm i.d.) with aqueous 65% methanol as mobile phase (1 ml/min) and detection at 254 nm.
Calibration graphs were linear from 19-508 and 30-900 ng, for I and II, respectively. Average
recoveries (n = 5) were 88.11+/-4.78 and 81.92+/-4.11%, respectively, for I and II. The method
was applied to the determination of I and II in fruits and cereals.
Record 20 of 57

TI: Novel approach to the "on-site" testing for sulfamethazine in pork carcasses.
AU: Shearan,-P; O'Keeffe,-M
AD: Natl. Food Centre, Dublin 15, Ireland
SO: Analyst (London). Dec 1994; 119(12): 2761-2764
AB: Porcine muscle was extracted by matrix solid phase dispersion (MSPD), as described by
Shearan et al. (FoodAddit. Contam., 1994, 11, 7). Elution of the analyte from the MSPD column
was effected with 8 ml CH2Cl2. Petroleum spirit (3 ml) was added to the eluate, which was then
loaded on to a 10 mg silica microcolumn, previously conditioned with 500 micro l of petroleum
spirit; elution was effected with 150 micro l methanol. A portion (40 micro l) of the eluate was
analysed by TLC on plates (10 x 10 cm) coated with silica gel 60, with a mobile phase of methanol
for the first run and ethyl acetate for the second run, and detection at 366 nm after spraying with
fluorescamine solution. The quantification limit was 30 ppb of sulfamethazine (sulphadimidine).
The method was used for the "on-site" detection of sulfamethazone residues in pork carcasses at
or below the maximum residue limit of 100 ppb.
Record 21 of 57

TI: Automated extraction of acetylgestagens from kidney fat by matrix solid-phase dispersion.
AU: Rosen,-J; Hellenas,-K-E; Tornqvist,-P; Shearan,-P
AD: Natl. Food Administration, 751 26 Uppsala, Sweden
SO: Analyst (London). Dec 1994; 119(12): 2635-2637
AB: Bovine kidney fat (0.5 g) was mixed with [3H]medroxyprogesterone acetate (internal standard)
ground to a thin film, blended with 2 g of Bondesil C18 (40 micro m; Varian) and packed into an
SPE column. The resulting matrix solid-phase dispersion (MSPD) column was loaded into a Gilson
ASPEC unit for automated washing and elution. A Bond-Elut C18 SPE column was also loaded
for further clean-up. The MSPD column was washed with 12 ml cyclohexane, dried with N2 and
gestagens were eluted with 8 ml aqueous 80% methanol. The eluate was diluted with H2O to
obtain a 50% methanol solution and applied to the activated Bond Elut column, which was washed
with 9.5 ml aqueous 50% methanol before elution was effected with 3.5 ml aqueous 80%
methanol. After evaporation, the extract was dissolved in 200 micro l aqueous 20% methanol for
liquid scintillation counting. Alternatively, portions (20 micro l) were screened using an EIA kit
(Ridascreen, Darmstadt, Germany). The recoveries of medroxyprogesterone acetate were 59% +/-
5%; similar results were obtained for chlormadinone acetate and megestrol acetate. The EIA
detection limits were 1-2 ng/g.
Record 22 of 57 ;

TI: Application of the matrix solid-phase dispersion technique for the determination of ivermectin
residues in fish muscle tissue.
AU: Iosifidou,-E; Shearan,-P; O'Keeffe,-M
AD: Aristotle Univ., Dept. Food Hygiene and Technol., School Vet. Med., 540 06 Thessaloniki,
Greece
SO: Analyst (London). Oct 1994; 119(10): 2227-2229
AB: Homogenized tissue (0.5 g) was blended with 2 g C18 end-capped packing material for 45 s.
The mixture was packed into a 10 ml syringe barrel and the resulting column was washed with 8 ml
hexane. Ivermectin (I) was eluted with 8 ml CH2Cl2/ethyl acetate (3:1) and the eluate was
evaporated to dryness under N2. The residue was dissolved in 1 ml methanol and the solution was
filtered. A 500 micro l portion of the filtrate was evaporated to dryness and 100 micro l 1-
methylimidazole/acetic anhydride/DMF (2:6:9) was added. The mixture was heated at 95degreeC
for 1 h, cooled and 1 ml CHCl3 was added. The solution was applied to a Sep-Pak silica cartridge
and the eluate collected. The column was washed with 9 ml CHCl3 and the eluate collected. The
combined eluates were evaporated to dryness and the residue was dissolved in 250 micro l
methanol. The solution was filtered and a 100 micro l portion of the filtrate was analysed by HPLC
on a Novapak C18 column (15 cm x 3.9 mm i.d.) with a micro Bondpak C18 guard column with
97% aqueous methanol as mobile phase (1 ml/min) and fluorescence detection (excitation and
emission wavelengths not given). The calibration graph was linear from 5-200 ng/ml of I. Intra- and
inter-assay RSD (n = 3 or 4) were 6.9-7.8 and 5.5-13.1%, respectively. Recoveries were >80%.
Record 23 of 57

TI: High-performance liquid-chromatographic analysis of sulfonamides in livestock products using
matrix solid-phase dispersion (MSPD) method with silica gel.
AU: Tamura,-H; Yotoriyama,-M; Kurosaki,-K; Shinohara,-N
AD: Tochigi Prefectural Inst. Public Health, Food Div., Tochigi 320, Japan
SO: Shokuhin-Eiseigaku-Zasshi. Jun 1994; 35(3): 271-275
AB: Sample (0.5 g) was mixed with 0.7 g silica gel and 0.5 g Na2SO4 in 1.5 ml acetonitrile then
dried and applied to a Bond Elut reservoir containing a bed of Na2SO4 with hexane for washing
and methanol or THF for elution (for analysis of meat or egg). The eluate was centrifuged at 4000
rpm for 2 min; the supernatant solution was evaporated to dryness. The residue was dissolved in
200 micro l methanol and then 10 micro l of the filtered solution was analysed by HPLC on a
column (15 cm x 4.6 mm i.d.) operated at 40degreeC with acetonitrile/1% acetic acid (9:41) as
mobile phase (1 ml/min) and detection at 272 nm. Detection limits for sulfameradine,
sulfadimidine, sulfamonomethoxine, sulfadimethoxine and sulfaquinoxarine were 0.01-0.04 ppm.
Recoveries were 69.6%-93.1%. The method was employed in assay of pork, chicken meat and
egg.
Record 24 of 57

TI: Extraction and liquid chromatographic analysis of sulfadimethoxine and 4-N-
acetylsulfadimethoxine residues in channel catfish (Ictalurus punctatus) muscle and plasma.
AU: Walker,-CC; Barker,-SA
AD: Louisiana State Univ., Lab. Residue Studies, Dept. Vet. Physiol., Pharm. and Toxicol., School
Vet. Med., Baton Rouge, LA 70803-8420, USA
SO: J-AOAC-Int. Nov-Dec 1994; 77(6): 1460-1466
AB: Muscle was extracted using matrix solid-phase dispersion (MSPD) and plasma with a modified
MSPD method in which 100 micro l plasma was vortex-mixed with 400 mg C18 in a disposable
chromatographic column. Analysis was by LC on a 5 micro m ODS Hypersil column (20 cm x 2.1
mm i.d.) with 0.017M-aqueous H3PO4 of pH 2.4/acetonitrile as mobile phase (71:29 for muscle
analysis and 73:27 for plasma analysis) as mobile phase (0.4 ml/min) and photodiode-array
detection set at 265 nm with a reference spectrum of 45 nm and a spectrum range of 210-320 nm.
A 10 micro l portion of muscle extract and a 25 micro l portion of plasma extract was used.
Recoveries were 79 and 67% for muscle and plasma, respectively. Detection limits were 26 ng
sulphadimethoxine and 26 ng acetyl sulphadimethoxine/g muscle and corresponding plasma
values were 33 and 11 ng/ml. Intra- and inter-assay RSD were
Record 25 of 57

TI: Preparation of milk samples for immunoassay and liquid chromatographic screening using
matrix solid-phase dispersion.
AU: Barker,-SA; Long,-AR
AD: Louisiana State Univ., Dept. Physiol., Pharmacol. and Toxicol., Baton Rouge, LA 70803-8420,
USA
SO: J-AOAC-Int. Jul-Aug 1994; 77(4): 848-854
AB: Sample (0.5 g) was blended with C18, internal standards or sample modifying agents (e.g.,
acids, bases, or chelators) for ~30 s. The semi-dry blend was applied to a 10 ml syringe barrel
containing a paper frit. The column head was covered with a filter paper disc and the contents
were compressed with a plunger to 4.5 ml. A disposable pipette tip on the end of the column
increased the residence time of eluting solvents on the column. Elution was effected with 9 ml of a
given solvent and 3-9 ml each of a series of solvents. The method can be used to increase the
specificity of drug immunoassays by fractionating any drugs that may cross-react. Specific drug
extraction and analysis procedures for several drugs used in dairy production are given. The
method can also be used for LC screening and confirmation of a suspect sample.
Record 26 of 57

TI: Solid phase techniques in the extraction of pesticides and related compounds from foods and
soils.
AU: Pico,-Y; Molto,-JC; Manes,-J; Font,-G
AD: Univ. Valencia, Lab. Toxicol., Fac. Farm., 46100 Burjassot, Valencia, Spain
SO: J-Microcolumn-Sep. Jul-Aug 1994; 6(4): 331-359
AB: A review is presented of the extraction of pesticides from milk, meat, sea-food, animal fat,
vegetable oils, lanolin, fruits, vegetables and soil. The techniques of solid-phase extraction, solid-
phase clean up and matrix solid phase dispersion are described. Tables are presented of the
extraction and clean up procedures and the pesticide extracted for 64 matrices with recoveries,
concentration ranges, detection limits, detectors used and references given. (97 references).
Record 27 of 57

TI: Matrix solid-phase dispersion as a multiresidue extraction technique for beta-agonists in bovine
liver tissue.
AU: Boyd,-D; O'Keeffe,-M*; Smythe,-R
AD: Natl. Food Centre, Dublin 15, Ireland
SO: Analyst (London). Jul 1994; 119(7): 1467-1470
AB: Salbutamol residues in bovine liver were determined at sub ppb level by combining matrix
sold-phase dispersion with RIA. Extraction was performed on a Sepralyte C18 column. A RIA kit
with antiserum raised against salbutamol and an EIA kit with antiserum raised against clenbuterol
were used. The scintillation cocktail was Cocktail T. Good recoveries of salbutamol were obtained
from 1-5 ppb. An enzyme hydrolysis procedure was optimized for deconjugating the residue
incurred. The method described was suitable for extracting and determining other beta-agonists
(sympathomimetics) such as clenbuterol, mabuterol, terbutaline and cimaterol at levels of
Record 28 of 57 ;

TI: Matrix solid-phase dispersion extraction and gas-chromatographic screening of polychlorinated
biphenyls in fish.
AU: Ling,-Y-C; Chang,-M-Y; Huang,-I-P
AD: Natl. Tsing Hua Univ., Dept. Chem., Hsinchu 30043, Taiwan
SO: J-Chromatogr-A. 27 May 1994; 669(1-2): 119-124
AB: Fillet of grass carp (0.5 g) was homogenized with 2 g of ODS silica (40 micro m), the mixture
was packed into a 5 ml column and analytes were eluted with hexane (10 ml). The eluate was
concentrated to 1 ml and a portion of the concentrate was injected on to a column (30 m x 0.53
mm i.d.) coated with DB-1 (1 micro m), operated with temp. programming from 170degreeC (held 3
min) to 300degreeC at 5degreeC/min with Ar/CH4 (19:1) as carrier gas (8 ml/min) and 63Ni ECD.
Alternatively analysis was performed by GC-MS on a column (30 m x 0.25 mm i.d.) coated with
DB-5 (0.25 micro m), operated with temp. programming from 70degreeC (held 5 min) to
180degreeC (held for 3 min) at 20degreeC/min, and then at 10degreeC/min to 320degreeC (held 6
min) and 70-eV EIMS. Test recoveries of various PCB at 0.6 ppm were evaluated. Mean
recoveries (n = 4) of main components were 89.1+/-2.0% for trichloro-PCB and 93.2+/-4.3% for
tetrachloro-PCB from KC-300 and 92.8 +/- 3.5% for pentachloro-PCB and 84.9 +/- 5.8% for
hexaclore-PCB from KC-500. Results are discussed.
Record 29 of 57 ;

TI: Comparison of matrix solid phase dispersion (MSPD) with a standard solvent extraction method
for sulphamethazine in pork muscle using high-performance liquid and thin-layer chromatography.
AU: Shearan,-P; O'Keeffe,-M; Smyth,-MR
AD: Natl. Food Centre, Dublin 15, Ireland
SO: Food-Addit-Contam. Jan-Feb 1994; 11(1): 7-15
AB: In the cited MSPD extraction/clean up procedure, pork tissue, unfortified or fortified with
sulphamethazine (I; sulphadimidine) at 0.05 and 0.1 micro g/g, was blended with C18 resin in a
mortar for 30-45 s. The blend was then packed into a syringe barrel, washed with hexane and
elution was effected with CH2Cl2. The purified extract was analysed (i) by HPLC on a stainless-
steel column (30 cm x 3.9 mm i.d.) of micro Bondapak C18 with a similar guard column, a mobile
phase (no flow rate given) of acetonitrile/10mM-ammonium acetate of pH 6.8 (1:3) and detection at
254 nm; and (ii) after solvent evaporation and reconstitution in methanol or after back extraction
with 0.01M-NaOH, by TLC on plates of silica gel 60 utilizing a modification of the Sulpha-on-Site
test system with detection by spraying with fluorescamine in acetone followed by visualization at
366 nm. The extracts were free from interferences and the recovery of I was >80%. Using HPLC
the calibration graph was linear for 0.025-1 micro g/ml of I and the detection limit was 0.025 micro
g/g. Residue levels found compared well with those obtained using a conventional extraction/silica
and C18 clean up method.
Record 30 of 57

TI: Matrix solid-phase dispersion extraction and the analysis of drugs and environmental pollutants
in aquatic species.
AU: Walker,-CC; Lott,-HM; Barker,-SA
AD: Louisiana State Univ., Lab. Residue Studies, School Veterinary Med., Baton Rouge, LA
70803, USA
SO: J-Chromatogr. 16 Jul 1993; 642(1-2): 225-242
AB: A review is presented of methods for the extraction and determination of drugs and chlorinated
pesticide residues in tissues of aquatic resources. Problems ocurring in the sample prep., isolation
and cleanup stages are discussed and future methods of residue analysis, viz., solid-phase
extraction, SFE and matrix solid-phase dispersion are described. (138 references).
Record 31 of 57

TI: Liquid-chromatographic analysis of antibacterial drug residues in food products of animal origin.
AU: Shaikh,-B; Moats,-WA
AD: Center Veterinary Med., Food and Drug Administration, Beltsville, MD 20705, USA
SO: J-Chromatogr. 23 Jul 1993; 643(1-2): 369-378
AB: A review is presented of recent developments in the LC determinations of antibiotic residues
(e.g., aminoglycosides, chloramphenicol, sulfonamides, tetracyclines, macrolides, beta-lactams
etc.) in food products of animal origin, e.g., meat or milk. Topics covered include cleanup
procedures such as ultrafiltration, liquid-liquid parition, solid-phase extraction, immunoaffinity and
matrix solid-phase dispersion as extraction, deproteination and concn. steps. (97 references).
Record 32 of 57

TI: Determination of sulphamethazine in animal tissues by enzyme immunoassay.
AU: Renson,-C; Degand,-G; Maghuin-Rogisster,-G; Delahaut,-P
AD: Univ. Liege, Lab. Anal. Denrees Aliment. Origin Animale, Fac. Med. Vet., 4000 Liege, Belgium
SO: Anal-Chim-Acta. 1 Apr 1993; 275(1-2): 323-328
AB: Muscle and liver from animals used for human consumption were prepared by matrix solid-
phase dispersion as previously described (Long Austin et al., J. Agric. Food Chem., 1990, 38,
423). Extracts or standard soln. (50 micro l) and sulphamethazine (I) - horse-radish peroxidase
conjugate (100 micro l) were incubated at 4degree overnight or at 37degree for 2 h in the wells of a
microtitre plate coated with rabbit anti-I antibodies. The wells were incubated with 5,5'-
tetramethylbenzidine soln. (150 micro l) at 37degree in the dark for 30 min, the reaction was
stopped by the addition of 6M-H2SO4 (50 micro l) and the absorbance was measured at 450 nm.
Recoveries were quantitative. Detection limits were 4.8 and 5.1 micro g kg-1 of I in muscle and
liver, respectively. Cross-reactivities (tabulated) were 0.1% with other sulphonamides except that
for sulphamerazine which was 13.2%.
Record 33 of 57

TI: Application of matrix solid-phase dispersion for the determination of clenbuterol in liver
samples.
AU: Boyd,-D; Shearan,-P; Hopkins,-JP; O'Keeffe,-M; Smyth,-MR
AD: Natl. Food Centre, Dublin 15, Eire
SO: Anal-Chim-Acta. 1 Apr 1993; 275(1-2): 221-226
AB: Liver was homogenized and mixed with [3H]clenbuterol. Portions (0.5 g) were mixed in a
mortar with Bondesil C18 (40 micro m; 2 g). The mixture was transferred to a syringe containing
two filter paper discs and the plunger was compressed to give a vol. of 4.5 ml. The material was
washed with hexane (8 ml) and H2O (8 ml), the excess of solvent was removed by applying
positive pressure and methanol (8 ml) was added. The first 1-ml portion of eluate was discarded,
the remaining eluate was evaporated to dryness at 55degree under N and the residue was
dissolved in ethanol (0.5 ml). Extracts (0.1 ml) were analysed by RIA carried out in tubes. Mixtures
were evaporated to dryness at 40degree under N, phosphate - gelatin buffer soln. (0.5 ml) was
added, the tubes were incubated at 37degree for 15 min and [3H]clenbuterol (0.1 ml) and
antiserum (0.1 ml) were added. After incubation at 37degree for 15 min and overnight at 4degree,
dextran - charcoal suspension (0.5 ml) was added and the tubes were centrifuged for 10 min at
1200 g. The supernatant soln. were decanted into phials and mixed with scintillation cocktail (10
ml) before liquid scintillation counting. The detection limit was 0.3 ng g-1 of clenbuterol in liver.
Inter- and intra-assay coeff. of variation were 16.1 to 19.3 and 4.9 to 8.9%, respectively.
Record 34 of 57

TI: Disruption and fractionation of biological materials by matrix solid-phase dispersion.
AU: Baker,-SA; Long,-AR; Hines,-ME
AD: Louisiana State Univ., Lab. Residue Stud., Dept. Physiol., Pharmacol. and Toxicol., Sch. Vet.
Med., Baton Rouge, LA 70803, USA
SO: J-Chromatogr. 15 Jan 1993; 629(1): 23-34
AB: A summary of data is presented on the application of matrix solid-phase dispersion to the
isolation of drug and pollutant residues from a variety of biological matrices, and its application to
the disruption and fractionation of muscle tissue, Mycobacterium paratuberculosis and Escherichia
coli.
Record 35 of 57

TI: Matrix solid-phase dispersion extraction and gas-chromatographic screening of 14 chlorinated
pesticides in oysters (Crassostrea virginica).
AU: Lott,-HM; Barker,-SA
AD: Louisiana State Univ., Lab. Residue Stud., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch.
Vet. Med., Baton Rouge, LA 70803, USA
SO: J-AOAC-Int. Jan-Feb 1993; 76(1): 67-72
AB: Oyster tissue, blended with delta-HCH as internal standard, was mixed with C18 silica and
transferred to a bed of activated Florisil. The resulting column was compressed before elution of
the pesticides with acetonitrile - methanol (9:1). A 2-micro l portion of the eluate was analysed by
GC on a column (30 m x 0.25 mm) coated with DB-5 (0.2 micro m) and operated with temp.
programming from 120degree (held for 2 min) at 10degree min-1 to 290degree (held for 4 min), N
as carrier gas (15 cm s-1) and ECD. Peak area ratios were used for quantitation. Typical
chromatograms obtained for oyster tissue fortified at 250 and 31.3 ng g-1 are reproduced, and
recoveries and inter- and intra-assay variabilities are reported for 14 pesticides. The eluate from
the extraction column was free from interfering co-extractives.
Record 36 of 57

TI: Matrix solid-phase dispersion linked to immunoassay techniques for the determination of
clenbuterol hydrochloride in bovine liver samples.
AU: Boyd,-D; Shearan,-P; Hopkins,-JP; O'Keeffe,-M; Smyth,-MR
AD: Natl. Food Centre, Dunsinea, Dublin 15, Eire
SO: Anal-Proc (London). Mar 1993; 30(3): 156-157
AB: Clenbuterol hydrochloride (I) was extracted by blending the liver sample with C18 and solvent
elution. The extracts were evaporated and the residues were dissolved in H2O for assay by using
an enzyme immunoassay kit (Riedel-de Haen, Darmstadt, Germany) in which I competed with the I
- peroxidase conjugate for binding to the antiserum and the final absorbance was measured at 410
nm. The kit had cross-reactivities of 71, 11, 10, 5.5 , 4.5 and 4% for mabuterol, salbutamol,
terbutaline sulphate, cimaterol, carbuterol hydrochloride and isoprenaline, respectively. Recovery
was satisfactory for 1 to 5 ng g-1 of added I, and results agreed well with those obtained by matrix
solid-phase dispersion - RIA.
Record 37 of 57

TI: Efficient biological analysis using MSPD [Matrix solid-phase dispersion].
AU: Barker,-S; Hawley-R
AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. Toxicol. Sch. Vet. Med., Baton Rouge,
LA, USA
SO: Int-Lab. Sep 1992; 22(8): 46, 48
AB: Rapid and simple drug determinations and immuno- or receptor assays can be carried out
using the matrix solid-phase dispersion technique for sample preparation. Samples are blended
with C18 sorbent followed by elution of analytes from the sample - C18 matrix. This microscale
method minimizes the amount of solvents used and steps necessary for analysis. Its application to
the determination of invermectin in beef liver is described.
Record 38 of 57

TI: Liquid-chromatographic confirmatory method for five sulfonamides in salmon muscle tissue by
matrix solid-phase dispersion.
AU: Reimer,-GJ; Suarez,-A
AD: CanTest Ltd., Vancouver, BC V6J IJ8, Canada
SO: J-AOAC-Int. Nov-Dec 1992; 75(6): 979-981
AB: Salmon muscle tissue was extracted by matrix solid-phase dispersion (details given), the
CH2Cl2 extracts were evaporated to dryness under N, the residue was washed with methanol, the
soln. was evaporated to dryness and the residue was dissolved in 200 micro l of methanol. A 20-
micro l portion of the soln. was analysed on a column (25 cm x 4.6 mm) of Supelcosil LC18-DB (5
micro m) with gradient elution with acetonitrile - 0.01M-ammonium acetate (pH 5.5) (details given)
with photodiode array detection. Calibration graphs were rectilinear from 60 to 5000 ppb. Intra-
assay coeff. of variation were generally 13% for sulfadiazine, sulfamerazine, sulfamethazine,
sulfadimethoxine and sulfapyridine. Detection limits were 48 to 150 ppb. Average recoveries were
66 to 82%.
Record 39 of 57

TI: Tissue drug residue extraction and monitoring by matrix solid-phase dispersion (MSPD) - HPLC
analysis.
AU: Barker,-SA; Long,-AR
AD: Louisiana State Univ., Lab. Residue Studies, Dept. Vet. Physiol., Pharmacol. and Toxicol.,
Sch. Vet. Med., Baton Rouge, LA 70803, USA
SO: J-Liq-Chromatogr. Aug 1992; 15(12): 2071-2089
AB: A summary is given of the methodology of matrix solid-phase dispersion in cleanup of drug
analytes extracted from tissues for determination by HPLC with UV or fluorimetric detection. The
procedure involves use of a column of blended derivatized silica (solid-phase support) and tissue
matrix for cleanup. The method is applied to several classes of drug.
Record 40 of 57

TI: Matrix solid-phase dispersion isolation and liquid chromatographic determination of oxolinic acid
in channel catfish (Ictalurus punctatus) muscle tissue.
AU: Jarboe,-HH; Kleinow,-KM
AD: Louisiana State Univ., Sch. Vet. Med., Dept. Vet. Physiol., Pharmacol. and Toxicol., Baton
Rouge, LA 70803, USA
SO: J-AOAC-Int. May-Jun 1992; 75(3): 428-432
AB: Muscle and bile containing piromidic acid (internal standard) were extracted on C18 columns.
Oxolinic acid (I) and its metabolites were eluted by sequentially washing with acetonitrile and
methanol. The eluates were combined, evaporated to dryness and the residue was reconstituted in
0.05M-acetic acid - methanol. A portion of the soln. was analysed by HPLC on a column (25 cm x
4.1 mm) of Versapack C18 (10 micro m) with gradient elution (1 ml min-1) with methanol and
anhyd. 0.05M-acetic acid (details given) and detection at 260 nm. The calibration graph was
rectilinear from 0.1 to 15 micro g g-1 of I and inter- and intra-assay coeff. of variation were 12.5 +/-
8.9 and 1.2%, respectively; recovery was 63 +/- 19.8 to 100.2 +/- 3.9%. The limit of detection was
0.05 micro g g-1.
Record 41 of 57

TI: Matrix solid-phase dispersion extraction and liquid-chromatographic determination of nicarbazin
in chicken tissue.
AU: Schenck,-FJ; Barker,-SA; Long,-AR
AD: US Food and Drug Admin., Baltimore, MD 21201, USA
SO: J-AOAC-Int. Jul-Aug 1992; 75(4): 659-662
AB: A column packed with the tissue sample blended with C18 material was washed with hexane
before nicarbazin was eluted with acetonitrile. After cleanup on alumina, it was determined on an
Econosphere (3 micro m) column (15 cm x 4.6 mm) with detection at 340 nm. Recoveries were
between 80.1 and 96.9% with coeff. of variation (n = 5) from 1.2 to 8.4%. The results are compared
with those obtained by the conventional ethyl acetate extraction method.
Record 42 of 57

TI: Matrix solid-phase dispersion extraction and liquid-chromatographic determination of ivermectin
in bovine liver tissue.
AU: Schenck,-FJ; Barker,-SA; Long,-AR
AD: US Food and Drug Admin., Baltimore, MD 21201, USA
SO: J-AOAC-Int. Jul-Aug 1992; 75(4): 655-658
AB: A column packed with a liver sample blended with C18 material was washed with hexane
before elution of ivermectin with CH2Cl2 - ethyl acetate (3:1). After cleanup on alumina it was
derivatized with DMF - acetic anhydride - 1-methylimidazole and determined on a column (25 cm x
4.6 mm) of Econosil C18 (5micro m) at 37degree with aq. 95% methanol as mobile phase (2 ml
min-1) and fluorimetric detection at 418 nm (excitation at 364 nm). Recoveries were between 72.1
and 77.4% for samples treated with 10 to 40 ng g-1, with coeff. of variation (n = 5) from 7.3 to
12.9%.
Record 43 of 57

TI: Analytical aspects of veterinary drug residues.
AU: Haagsma,-N
AD: Unvi. Utrecht, Dept. Sci. Food and Animal Origin, Fac. Vet. Med., 3508 TD Utrecht,
Netherlands
SO: Mikrochim-Acta. 1991; II(1-6): 63-70
AB: A review is presented, with 88 references, of recent developments in the determination of
veterinary drug residues in food of animal origin. The application of solid-phase extraction,
immunoaffinity and matrix solid-phase dispersion as rapid clean-up and concentration techniques
is discussed. Automated methods, e.g., immunoassays and fully automated sample treatment LC,
are also discussed.
Record 44 of 57

TI: Determination of aminoglycoside antibiotics by reversed-phase ion-pair high-performance liquid
chromatography coupled with pulsed amperometry and ion-spray mass spectrometry.
AU: McLaughlin,-LG; Henion,-JD
AD: Cornell Univ., Drug Testing and Toxicol., NYS Coll. Vet. Med., Ithaca, NY 14850, USA
SO: J-Chromatogr. 7 Feb 1992; 591(1-2): 195-206
AB: Various stationary phases, mobile phase compositions and ion-pairing ions were evaluated for
the cited detemination. Bovine tissues were extracted by matrix solid-phase dispersion as
previously described (Schenck, US FDA Laboratory Information Bulletin, Vol. 7, Issue 4, No 3559).
Best results were obtained by using a column (10 cm x 4.6 mm) of Spherisorb ODS-2 (3 micro m)
with 8% acetontrile in 20mM-pentafluoropropionic acid as mobile phase. With pulsed amperometric
detection at 0.1 V and a pulse duration of 480 ms, detection limits were in the ng range. For MS
detection an ion-spray interface was used and MS was carried out with a triple quadrupole
instrument equipped with an atmospheric pressure ion source in the positive ion mode. Selected-
ion monitoring was at m/e 351, 265, 301 and 293 for spectinomycin, hygromycin B, steptomycin
and dihydrostrptomycin, respectively. Detection limits were in the low ng range.
Record 45 of 57 ;

TI: Matrix solid-phase dispersion (MSPD) extraction and gas-chromatographic screening of nine
chlorinated pesticides in beef fat.
AU: Long,-AR; Soliman,-MM; Barker,-SA
AD: Louisiana State Univ., Dept. Vet. Physiol., Sch. Vet. Med., Baton Rouge, LA 70803, USA
SO: J-Assoc-Off-Anal-Chem. May-Jun 1991; 74(3): 493-496
AB: Beef fat (0.5 g) containing nine chlorinated pesticides (e.g., heptachlor, aldrin, dieldrin, endrin,
pp'-DDT) and fortified with dibutyl chlorendate (internal standard; 25 micro g ml-1) was blended
with 2 g of C18 (octadecylsilyl-derivatized silica; 40 micro m) and the homogeneous matrix blend
was transferred to a column containing activated Florisil. The pesticides were eluted with 8 ml of
acetonitrile and a 0.2-micro l portion of the eluate was analysed by GC on a column (25 m x 0.25
mm) of DB-5 (0.2 mm) with temp. programming from 120degree (held for 2 min) to 290degree
(held for 2 min) at 10degree min-1, N as carrier gas (14 cm s-1) and ECD. Calibration graphs were
rectilinear and mean intra- and inter-assay coeff. of variation were 2.5 to 5.1 and 6 to 14%,
respectively. Recoveries ranged from 85 to 102% and co-extractants did not interfere.
Record 46 of 57

TI: Multi-residue matrix solid-phase dispersion (MSPD) extraction and gas-chromatographic
screening of nine chlorinated pesticides in catfish (Ictalurus punctatus) muscle tissue.
AU: Long,-AR; Crouch,-MD; Barker,-SA
AD: Louisiana State Univ., Sch. Vet. Med., Dept. Vet. Physiol., Pharmacol. and Toxicol., Baton
Rouge, LA 70803, USA
SO: J-Assoc-Off-Anal-Chem. Jul-Aug 1991; 74(4): 667-670
AB: Fish muscle tissue (0.5 g) was blended into octadecylsilyl derivatized C18 silica (40 micro m)
packing until homogenized. The blend was packed into a column containing 2 g of activated
Florisil and pesticides were eluted with acetonitrile. A portion of the extract was analysed by GC on
a column (25 m x 0.25 mm) of DB-5 (0.2 mm) with temp. programming from 120degree (held for 2
min) to 290degree (held for 5 min) at 10degree min-1, N as carrier gas (14 cm s-1) and ECD at -
0.24 mV. Calibration graphs were rectilinear and intra- and inter-assay coeff. of variation ranged
from 1.8 to 4.7% and from 5.0 to 16.9%, respectively; recoveries were >=77.2%. A theoretical
detection limit of ~10 ng g-1 was obtained by extrapolation of the data.
Record 47 of 57

TI: Matrix solid-phase dispersion (MSPD) isolation and liquid-chromatographic determination of
furazolidone in pork muscle tissue.
AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA
AD: Louisiana State Univ., Dept. Vet. Physiol., Sch. Vet. Med., Baton Rouge, LA 70803, USA
SO: J-Assoc-Off-Anal-Chem. Mar-Apr 1991; 74(2): 292-294
AB: Pork muscle tissue (0.5 g) was homogenized with C18 (18% load; endcapped; 2 g). A column
was made from the C18 - pork matrix which was washed with hexane (8 ml) before elution with
ethyl acetate. The eluate was passed through a pre-washed activated alumina column and dried
under N. The residue was mixed with 0.1 ml each of methanol and 0.015M-H3PO4 and the mixture
was sonicated for 5 to 10 min then centrifuged at 17,000 g for 5 min. The clear supernatant was
analysed by HPLC on a column (30 cm x 4 mm) of ODS (10 micro m), operated at 45degree, with
a mobile phase (1 ml min-1) of 0.015M-H3PO4 - acetonitrile (3:2) and detection at 365 nm. The
calibration graph was rectilinear and the average recovery was 89.5% for 7.8 to 250 ng g-1 of
furazolidone. The detection limit was 390 pg and the inter- and intra-assay coeff. of variation were
9.9 and 1.5%, respectively.
Record 48 of 57 ;

TI: Matrix solid-phase dispersion isolation and liquid-chromatographic determination of
sulphadimethoxine in catfish (Ictalurus punctatus) muscle tissue.
AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA
AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton
Rouge, LA 70803, USA
SO: J-Assoc-Off-Anal-Chem. Nov-Dec 1990; 73(6): 868-871
AB: A 0.5-g portion of fish muscle tissue was blended with 2 g of C18 material (Analytichem
International) and methanolic sulphamethoxazole (internal standard) and packed into a 10-ml
column, followed by washing with hexane and elution with 8 ml of CH2Cl2. The eluate was
evaporated at 40degree in a stream of N, and the residue was dispersed in 0.5 ml of mobile phase.
The suspension was centrifuged and a portion (25 micro l) of the supernatant soln. was analysed
by HPLC on a MicroPak ODS (10 micro m) column (30 cm x 4 mm) with a mobile phase (1 ml min-
1) of 17mM-H3PO4 - acetonitrile (13:7) and diode-array detection at 270 nm. Sulphadimethoxine
and the internal standard were well separated, and calibration graphs of peak-area ratios were
rectilinear up to 1.6 micro g g-1; the detection limit was 50 ng g-1.
Record 49 of 57 ;

TI: Matrix solid-phase dispersion isolation and liquid-chromatographic determination of
oxytetracycline in catfish (Ictalurus punctatus) muscle tissue.
AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA
AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton
Rouge, LA 70803, USA
SO: J-Assoc-Off-Anal-Chem. Nov-Dec 1990; 73(6): 864-867
AB: A 0.5-g portion of fish muscle tissue was blended with a mixture of 2 g of C18 material
(Analytichem International) and 0.05 g each of EDTA and oxalic acid and packed into a 10-ml
column, followed by washing with hexane and elution of oxytetracycline (I) with 8 ml of 0.06% t-
butyl-4-methoxyphenol - 0.06% 2,6-di-t-butyl-p-cresol in acetonitrile - methanol (1:1). The eluate
was evaporated at 40degree in a stream of N, and the residue was dispersed in 0.5 ml of mobile
phase. The suspension was centrifuged and the supernatant soln. (25 micro l) was injected on to a
MicroPak ODS (10 micro m) column (30 cm x 4 mm) with a mobile phase (1 ml min-1) of 0.02M-
oxalic acid - acetonitrile - methanol (28:11:1) and diode-array detection at 365 nm. Calibration
graphs of peak area were rectilinear up to 3.2 micro g g-1 of I; the detection limit was 50 ng g-1.
Record 50 of 57 ;

TI: Matrix solid-phase dispersion isolation and liquid-chromatographic determination of five
benzimidazole anthelmintics in fortified beef liver.
AU: Long,-AR; Malbrough,-MS; Hsieh,-LC; Short,-CR; Barker,-SA
AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton
Rouge, LA 70803, USA
SO: J-Assoc-Off-Anal-Chem. Nov-Dec 1990; 73(6): 860-863
AB: A 0.5-g portion of liver was added to 2 g of C18 material (Analytichem International), a mixture
of albendazole, fenbendazole, oxfendazole, thiabendazole and mebendazole (internal standard)
was added. The mixture was blended, packed into a 10-ml column,followed by washing with
hexane and elution of the benzimidazoles with 8 ml of acetonitrile. The eluate was purified by
passage through an alumina column and evaporated in a stream of N, and the residue was
dispersed in 0.1 ml of methanol plus 0.4 ml of 17mM-H3PO4. The suspension was centrifuged, the
supernatant soln. was filtered (0.45 micro m), and a 20-micro l portion of the filtrate was injected on
to a MicroPak ODS (10 micro m) column (30 cm x 4 mm) operated with 17mM-H3PO4 -
acetonitrile (3:2) as mobile phase (1 ml min-1) and diode-array detection at 290 nm. The calibration
graphs of peak area were rectilinear up to 3.2 micro g g-1 of the four analytes; the detection limit
was 0.1 micro g g-1.
Record 51 of 57

TI: Quantitative method for the detection of sulphonamide residues in meat and milk samples with
a high-performance thin-layer-chromatographic method.
AU: Van-Poucke,-LSG; Depourcq,-GCI; Van-Peteghem,-CH
AD: State Univ. Ghent, Lab. Pharm. Microbiol. and Hyg., 9000 Ghent, Belgium
SO: J-Chromatogr-Sci. Oct 1991; 29(10): 423-427
AB: A high-performance TLC method for the separation and detection of sulphonamides after
solid-phase extraction for meat samples and a modified matrix solid-phase dispersion extraction for
milk is described. The extracts were applied to Kieselgel 60 F254 plates which were developed for
30 min in a saturated chamber with a three-multiple development system with methanol (containing
2% ammonia) - CH2Cl2 (30:70, 15:85 and 5:95) to successive distances of 15, 30 and 45 mm,
respectively. The calibration graph was rectilinear for 0.5 to 40 mg of the six sulphonamides tested;
the limit of quantification was 4 micro g kg-1.
Record 52 of 57

TI: Veterinary drug residues in meat - possibilities of their analytical determination.
AU: Petz,-M
AD: Bergische Univ. GH, Lehrstuhl Lebensmittelchem., 5600 Wuppertal, Germany
SO: Mitt-Geb-Lebensmittelunters-Hyg. 1991; 82(1): 7-23
AB: A review is presented, with 43 references. The most recently proposed limits for veterinary
drugs in animal tissues, milk and eggs (FAO/WHO 1990) are tabulated and the results of recent
surveys are discussed. Suitable screening tests and methods of determination are described.
Newer methods of separation from the matrix, e.g., matrix solid-phase dispersion, immunoaffinity
chromatography, are given special attention.
Record 53 of 57

TI: Matrix solid-phase dispersion (MSPD) isolation and liquid-chromatographic determination of
clorsulon in milk.
AU: Schenck,-FJ; Barker,-SA; Long,-AR
AD: Food and Drug Admin., Baltimore, MD 21201, USA
SO: J-Liq-Chromatogr. Sep 1991; 14(15): 2827-2834
AB: Milk (0.5 g) was blended with C18 packing material (2 g) and the mixture was loaded into an
empty syringe barrel fitted with a frit. The column was washed with hexane (3 ml), the eluate was
discarded and the column was attached to a Florisil solid phase extraction cartridge. The tandem
columns were eluted with ethyl ether (3 x 3 ml), the C18 column was removed and clorsulon (I)
was eluted from the Florisil column with 2 ml of ether. The eluate was evaporated to dryness, the
residue was dissolved in mobile phase (1 ml) and the soln. was filtered. A portion (200 micro l) of
the filtrate was analysed by HPLC on a column (15 cm x 4.6 mm) of Econosphere (3 micro m) with
a mobile phase (1 ml min-1) of acetonitrile - phosphate buffer soln. of pH 7 (1:3) and detection at
265 nm. Recoveries were 88.8 to 96.6% for 50 to 200 ppm of I with coeff. of variation of 2.7 to
7.9%.
Record 54 of 57

TI: Matrix solid-phase dispersion (MSPD) extraction and liquid-chromatographic determination of
five benzimidazole anthelmintics in pork muscle tissue.
AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA
AD: Louisiana State Univ., Dept. Vet. Physiol. Pharmacol. and Toxicol., Sch. Vet. Med., Baton
Rouge, LA 70803, USA
SO: J-Food-Compos-Anal. Mar 90; 3(1): 20-26
AB: Tissue was blended (1:4) with 18% ODS silica (40 micro m) and the blend was packed into a
10-ml plastic syringe barrel and washed with hexane before elution of albendazole (I),
fenbendazole (II), oxfendazole (III) and thiabendazole (IV) with acetonitrile. The eluate was
cleaned up by passage through a column of activated alumina and a portion was analysed by
HPLC on a column (30 cm x 4 mm) of ODS silica (10 micro m) at 45degree with aq. 17mM-H3PO4
- acetonitrile (3:2) as mobile phase (1.0 ml min-1) and detection at 290 nm vs. mebendazole as
internal standard. Recoveries of 0.1 to 3.2 mg g-1 were 86 to 104% for I, 92 to 105% for II, 78 to
101% for III and 73 to 93% for IV, with mean coeff. of variation of 6.4, 5.5, 7.9 and 7.2%,
respectively.
Record 55 of 57

TI: Matrix solid-phase dispersion (MSPD) isolation and liquid-chromatographic determination of
oxytetracycline, tetracycline and chlortetracycline in milk.
AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA
AD: Louisiana State Univ., Dept. Vet. Physiol. Pharmacol. and Toxicol., Sch. Vet. Med., Baton
Rouge, LA 70803, USA
SO: J-Assoc-Off-Anal-Chem. May-Jun 1990; 73(3): 379-384
AB: Milk (0.5 ml) was mixed with 2 g of C18 silica, 0.05 g of Na2EDTA and 0.05 g of oxalic acid,
with gentle grinding to give a homogeneous mixture. The resulting material was packed into a
column (10-ml plastic syringe) and washed with hexane (8 ml). The cited drugs were eluted with
ethyl acetate - acetonitrile (1:3; 8 ml), the solvent was evaporated, and the residue was dissolved
in mobile phase for HPLC analysis. This was performed on a column (30 cm x 4 mm) of Micro Pak
ODS (10 micro m), with 10mM-oxalic acid - acetonitrile (7:3) at 40degree as mobile phase (1 ml
min-1) and detection at 365 nm. Calibration graphs were rectilinear for 100 to 3200 ng ml-1, and
recoveries were 63.5 to 93.3%. Inter- and intra-assay coeff. of variation (n = 5) were 8.5 to 20.7%
and 1.0 to 9.3%, respectively.
Record 56 of 57 ;

TI: Method for the isolation and liquid-chromatographic determination of chloramphenicol in milk.
AU: Long,-AR; Hsieh,-LC; Bello,-AC; Malbrough,-MS; Short,-CR; Barker,-SA
AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton
Rouge, LA 70803, USA
SO: J-Agric-Food-Chem. Feb 1990; 38(2): 427-429
AB: A modification of the matrix solid-phase dispersion extraction method of Barker et al. (Anal.
Abstr., 1990, 52, 5D21) was applied in the determination of chloramphenicol (I) in cow`s milk. The
extracts were analysed by HPLC on a Varian MCH-10 (10 micro m) column (30 cm x 4 mm) at
35degree with 17mM-H3PO4 - acetonitrile (13:7) as mobile phase (1 ml min-1) and photodiode-
array detection at 278 nm. The calibration graph was rectilinear from 62.5 to 2000 ng ml-1 of I and
recoveries were from 60.8 to 79.0%. Inter- and intra-assay coeff. of variation were 11.6 (n = 30)
and 1.4% (n = 5), respectively.
Record 57 of 57 ;

TI: Multi-residue method for the determination of sulphonamides in pork tissue.
AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA
AD: Louisana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton
Rouge, LA 70803, USA
SO: J-Agric-Food-Chem. Feb 1990; 38(2): 423-426
AB: A modification of the matrix solid-phase dispersion extraction method of Barker et al. (Anal.
Abstr., 1990, 52, 5D21) with CH2Cl2 as eluent was applied in the determination of sulphadiazine,
sulphadimethoxine, sulphadimidine, sulphafurazole, sulphamethizole, sulphanilamide and
sulphathiazole in pork (0.5 g). The extracts were analysed by HPLC on a Varian MCH-10 column
(30 cm x 4 mm) at 40degree with 17mM-H3PO4 - acetonitrile (7:3) as mobile phase (1 ml min-1)
and photodiode-array detection at 270 nm. Sulfamerazine was used as internal standard.
Calibration graphs were rectilinear from 62.5 to 2000 ng g-1 of each sulphonamide and detection
limits were from 31.3 to 62.5 ng g-1. Inter- and intra-assay coeff. of variation were 7.2 to 13.3% (n
= 30) and 3.5 to 6.2% (n = 5), respectively. Recoveries were from 70.4 to 95.8%. The method is
simple, yields interference-free extracts and may be applied to other tissues or matrices.

Source: http://www.weber.hu/PDFs/SPE/MSPD_refs.pdf

Research interests

2013: Alt A, Hilgers R-D, Tura A, Nassar K, Schneider T, Hüber A, Januschowski K, Grisanti S, Lüke J, Lüke M (2013) The Neuroprotective Potential of Rho-Kinase Inhibitioin in Promoting Cell Survival and Reducing Reactive Gliosis in Response to Hypoxia in Isolated Bovine Retina. Cell Physiol Biochem 32: in press. Rassaei M, Thelen M, Abumuaileq R, Hescheler J, Luke M, Schneider T (2013) Ef

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Dr. med. Friedemann Lindmayer Facharzt für Kinderheilkunde und Notfallmedizin Leitender Notarzt im Rettungsdienstbereich Karlsruhe Diagnostik – Segen und Fluch Verhaltensauffälligkeiten bei Kindern mit Entwicklungsstörungen Etwa 1/3 der behinderten Kinder haben gleichzeitig Verhaltensauffälligkeiten. Dies reicht von lautem Schreien, dissozialen Verhaltensweisen bis zu schwerem frem

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