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Research Article
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Uma et al /International Journal of Pharmaceutical Sciences Letters 2012 Vol. 2 (1)| 10-11
Development and Validation of LCMS Method for the Estimation of
Pramipexole in Human Plasma
G.Uma*, M.Manimala1, M.Vasudevan1, S.Karpagam2 and Deecarman2
* Department of Pharmaceutics, C. L. Baid Metha College of pharmacy, Chennai-97 Tamilnadu, India. 1Roxanne Research private limited, Taramani Chennai -113, Tamilnadu, India. 2Dr.M.G.R.University Chennai - 600095 ABSTRACT:
An accurate and precise LCMS method was developed for the determination of pramipexlole in hu-
man plasma.
Method: Separation of the drug was achieved on Hypersil gold column using a mobile phase consisting of Ace-
tonitrile : Ammonium Formate (65:35). Quetiapine Fumarate was used as an internal standard. Solid Phase extrac-
tion technique was used for pramipexole using Strata-X 33 µ m cartridges. Samples were ionized by positive-ion
electro spray ionization mode. The mass transitions m/z 212.00 to 153.00 and 384.700 to 220.300 were used to
measure Pramipexole and Quetiapine Fumarate respectively. The assay was calibrated over the range 20 to 4000
pg/ml with correlation coefficient of 0.9928.
Results: Validation data showed were within the limits. No matrix effect was found in different sources of human
plasma tested. Mean extraction recovery of pramipexole was satisfactory.
Experimental Methods
Chemicals and reagents
Pramipexole is a non-ergoline dopamine agonist Methanol and Acetonitrile of HPLC grade from indicated for treating early-stage of Parkinson’s disease Merck, Water (HPLC Grade), Ammonium Formate and restless legs syndrome. It is also sometimes used off- AR Grade, Pramipexole dihydrochloride monohy- label as a treatment for cluster headache and to counteract drate from Orchid Chemicals & pharmaceuticals Ltd, the problems with sexual dysfunction experienced by India. Quetiapine Fumarate from Lupin Limited, Ma- some users of the selective serotonin reuptake inhibitor harashtra, India. antidepressants. Pramipexole has shown robust effects on Instrumentation and chromatographic conditions pilot studies in a placebo-controlled proof of concept The mass spectroscopic detection was performed on study in bipolar disorder. It is also being investigated for API 5500 using electrospray positive ionization. The the treatment of clinical depression and fibromvalgia. For chromatography was performed on a Hypersil gold the determination of Pramipexole HPLC, LCMS and GC- column using a mobile phase consisting of Acetoni- MS methods1-4 have been reported. Some of these meth- trile : Ammonium Formate (65:35). Quetiapine Fu- ods use complicated extraction instruments, long and marate was used as an internal standard. Chroma- tedious extraction procedures and large amounts of sol- tograms were acquired using the computer based Ana- vents or biological fluids for extraction. The main objec- lyst Software version 1.4.2.supplied by applied biosci- tive of this work is to develop rapid, selective and sensi- ence and the data were processed by peak area ratio. tive LC-MS / MS methods that have short and simple The ion spray potential was set at 5500 kV and the extraction procedures, consume small amounts of solvent source of temperature was 500oC. The collision acti- and biological fluid for extraction and a short turn-around vation dissociation (CAD) gas was setting at 10; Ni- trogen was used as collision gas. The mass spectrome-ter was used in positive ion mode and multiple reac-tion monitoring (MRM) using turbo ion spray ioniza- Key words: Pramipexole, Human plasma, LC-MS-MS
tion mode as an interface. The transition m/z 212.00 → 153.00 was monitored for pramipexole and the Received 18 December 2011; received in revised form 28 transition m/z 384.70 → 220.300 for quetiapine on a
*Corresponding Author: G.Uma,, Department of Pharma-
Preparation of calibration curve (CC) standards and ceutics, C. L. Baid Metha College of pharmacy, Chennai-97 quality control (QC) samples A stock solution of pramipexole and quetiapine (1mg/ Email: umagok@yahoo.com.
mL) were prepared in methanol. Calibration standards Uma et al /International Journal of Pharmaceutical Sciences Letters 2012 Vol. 2 (1)| 10-11
were prepared by spiking blank plasma with Pramipex- 107.56, 98.94, 104.11 and 102.09 % respectivelyThe ole to get the concentration of 20.2400, 40.4800, results obtained from measurement of linearity, preci-84.3320, 276.5000, 737.3340, 1474.6660, 2949.3300 sion and accuracy are listed in Table 1 and 2. Recovery and 3932.4400 Pg/mL. Quality control samples were of Pramipexole was evaluated by comparing mean ana- prepared by spiking blank plasma with 20.3960, 55.1220, 1469.932 and 2939.8640 Pg/mL of pramipex- lyte responses of six processed samples of low (LQC), ole. The stock solutions were stored at 4-80 C. medium (MQC) and high (HQC) quality control samples Table 1: Concentration of pramipexole in calibration stan- to mean analyte responses of six appropriately diluted
dards prepared in human plasma
pure diluted solutions. Mean recovery values are 74.03, 82.52 and 80.12 % at low, medium and high quality control levels respectively. Mean recovery value for the internal standard was 80.43% and it is within the limit. REFERENCES
[1] Malenovic A, Janic-stojanovic B, Vemic A, Ivanovic
D and Medenica M, JAOAC Int.2010, 93,1102 .
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methanol. Then 500µl sample (Analyte + IS) was [6] Hartmann C, Smeyers-Verbeke J , Massart D L and added to it. It was washed with 1 mL of water two McDowall R.D, J. Pharmaceut. Biomed. Anal. 1998, 17,
times followed by 1 mL of 20% methanol in water. 193. Finally it was eluted with 500µl of methanol and dried [7] The European Agency for the Evaluation of Medicinal the samples under N2 and reconstituted the samples Products, 2001, http://www.eudra.org/emea.html. with 300 µL of Mobile phase, vortexed for 1 minute [8] U.S. Department of Health and Human Services, Food and 2 µ L of the sample was injected. The developed and Drug Administration, 2001, http://www.fda.gov/cvm. method was validated in accordance with current ac- [9] Guidance for Industry, Bioanalytical Method Valida- tion, Food and Drug Administration, May 2001 RESULTS AND DISCUSSION
The assay was found to be linear for pregabalin con-centrations in the range 20 to 4000 pg/mL . The preci- Cite this article as: G.Uma, M.Manimala, M.Vasudevan,
sion and accuracy were studied satisfactory at four QC S.Karpagam and Deecarman. Development and Validation of concentrations for pramipexole. The intraday precision LCMS Method for the Estimation of Pramipexole in Human and accuracy of the method at QC levels (20.3960 pg/ Plasma. Int. J. Pharm. Sci. Letters. 2012 ; 2 ; (1) 10 –11
ml, 55.1220 pg/ml, 1469.9320 pg/ml and 2939.8640
pg/ml (n = 6) were 16.97, 13.80, 3.01 and 2.26% and Source of Support: Nil. Conflict of interest: None declared.
96.05, 105.08, 103.42 and 100.17 % respectively. The
interday precision and accuracy of the method at QC
levels (n=6) were 20.31, 18.54, 3.30 and 5.57 and

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