Bokka Ramesh, Nemali Manjula, Sistla Ramakrishna, Potturi Sita Devi. Direct injection HILIC-MS/MS analysis of darunavir in rat plasma applying supported liquid extraction[J]. Journal of Pharmaceutical Analysis, 2015, (1): 43-50. doi: 10.1016/j.jpha.2014.05.001
Citation:
Bokka Ramesh, Nemali Manjula, Sistla Ramakrishna, Potturi Sita Devi. Direct injection HILIC-MS/MS analysis of darunavir in rat plasma applying supported liquid extraction[J]. Journal of Pharmaceutical Analysis, 2015, (1): 43-50. doi: 10.1016/j.jpha.2014.05.001
Bokka Ramesh, Nemali Manjula, Sistla Ramakrishna, Potturi Sita Devi. Direct injection HILIC-MS/MS analysis of darunavir in rat plasma applying supported liquid extraction[J]. Journal of Pharmaceutical Analysis, 2015, (1): 43-50. doi: 10.1016/j.jpha.2014.05.001
Citation:
Bokka Ramesh, Nemali Manjula, Sistla Ramakrishna, Potturi Sita Devi. Direct injection HILIC-MS/MS analysis of darunavir in rat plasma applying supported liquid extraction[J]. Journal of Pharmaceutical Analysis, 2015, (1): 43-50. doi: 10.1016/j.jpha.2014.05.001
Natural Products Chemistry Division, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500607, India
Medicinal Chemistry & Pharmacology Division, Indian Institute of Chemical Technology, Tarnaka
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The authors are grateful to Dr. M. Lakshmi Kantam, Director, CSIR-IICT for providing facilities to perform this work. B. Ramesh is grateful to UGC for the award of Senior Research Fellowship and Osmania University for Ph.D. registration
A novel bioanalytical method was developed and validated for the quantitative determination of darunavir (DRV) in rat plasma by employing hydrophilic interaction chromatography and tandem mass spectrometry (HILIC–MS/MS) with supported liquid extraction (SLE). Irbesartan (IRB) was used as an internal standard (IS). The analyte in rat plasma (200 mL) was isolated through SLE using ethyl acetate as the eluting solvent. The chromatographic separation was achieved on Luna-HILIC (250 mm4.6 mm, 5 μm) column with a mobile phase of 0.1% of formic acid in water:acetonitrile (5: 95, v/v), at a constant flow rate of 1.0 mL/min. The MS/MS ion transitions for DRV (548.1-392.0) and IS (429.2-207.1) were monitored on an ion trap mass spectrometer, operating in the multiple reaction monitoring (MRM) mode. The lower limit of quantitation (LLOQ) was 0.2 ng/mL and quantitation range was 0.2–5000 ng/mL. The method was validated for its selectivity, sensitivity, carryover, linearity, precision, accuracy, recovery, matrix effect and stability. The method was successfully applied to pharmacokinetic study in rats.
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