Bioanalytical Method Development and Validation for Simultaneous Estimation of (R) - and (S) - Isomer of S002-333: a potent Novel Anti-Thrombotic Agent using LC-MS/MS
IR@CDRI: CSIR-Central Drug Research Institute, Lucknow
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| Creator |
Bhatta, R S
Chhonker, Y S Kumar, D Saxena, A K Jain, G K |
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| Date |
2012-08-08T12:11:43Z
2012-08-08T12:11:43Z 2011 |
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| Identifier |
Medicinal Chemistry Research , 2011, 20(9), 1581-1588
http://hdl.handle.net/123456789/871 |
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| Description |
A selective, sensitive and high throughput liquid chromatography–tandem mass spectrometry (LC–MS/MS) method has been developed and validated for the chromatographic separation and quantitation of diastereomers of S002-333, a novel anti-thrombotic agent in rabbit plasma. Sample clean-up involved liquid–liquid extraction (LLE) of both the isomers and internal standard (β-carbolinamide) from 200µl of rabbit plasma. Both the analytes were chromatographically separated on a chiralcell OJ-RH column (150 ×4.6mm, 5µ particle size) using a gradient flow program comprising of 0.1% formic acid, methanol and acetonitrile as the mobile phase. The parent→product ion transitions (MRM) for both the isomers and IS were 386.4 →214.2 m/z and 216.1→144.2 m/z respectively, were monitored on a triple quadrupole mass spectrometer, operating in positive ion mode. The MS/MS response was linear over the concentration range from 1.56 ng/mL to 400 ng/ml, with a lower limit of detection (LOD) was 1.56 ng/ml. The intra- and inter-day precisions (% R.S.D.) between 3.96 to 13.80 for both analytes and the accuracies (% bias) were between -4.05 to 5.93. The validated method can be used in most or all stages of the screening and optimizing process for pharmacokinetic and toxicokinetics studies.
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1315851 bytes
application/pdf |
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| Language |
en
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| Relation |
CDRI Communication No. 7954
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| Subject |
LC-MS-MS
Bioanalytical Diastereomers Pharmacokinetics Chiral chromatography |
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| Title |
Bioanalytical Method Development and Validation for Simultaneous Estimation of (R) - and (S) - Isomer of S002-333: a potent Novel Anti-Thrombotic Agent using LC-MS/MS
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Article
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