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Direct injection HILIC-MS/MS analysis of darunavir in rat plasma applying supported liquid extraction

Journal of Pharmaceutical Analysis 2015年第1期5卷 43-50页

作者： Bokka Ramesh Nemali Manjula Sistla Ramakrishna potturi sita devi Natural Products Chemistry Division Indian Institute of Chemical TechnologyTarnakaHyderabad 500607India Medicinal Chemistry & Pharmacology Division Indian Institute of Chemical TechnologyTarnakaHyderabad 500607India

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）.lrbesartan（IRB） was used as an internal standard（IS）.The analyte in rat plasma（200 μL） was isolated through SLE using ethyl acetate as the eluting *** chromatographic separation was achieved on Luna-HILIC（250 mm × 4.6 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 1.0mL/*** 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） *** lower limit of quantitation（LLOQ） was 0.2 ng/mL and quantitation range was 0.2-5000 ng/*** method was validated for its selectivity,sensitivity,carryover,linearity,precision,accuracy,recovery,matrix effect and *** method was successfully applied to pharmacokinetic study in rats.

关键词： Darunavir HILIC-MS/MS Rat plasma Supported liquid extraction

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LC–HRMS determination of piperine on rat dried blood spots: A pharmacokinetic study

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Journal of Pharmaceutical Analysis 2016年第1期6卷 18-23页

作者： Bokka Ramesh P. Rajesh Rao Vadaparthi Genji Sukumar Nemali Manjula Katragadda Suresh Babu potturi sita devi Natural Products Chemistry Division Indian Institute of Chemical Technology Tarnaka Hyderabad 500607 India

A liquid chromatography-high resolution mass spectrometry （LC-HRMS） method was developed and validated for the determination of piperine （PPR） on dried blood spots （DBS）. DBS samples were prepared by spiking the whole blood with analyte to produce 30 μL of blood spots on specimen collection cards. Chromatographic separation was achieved on an Atlantis dC18 column using acetonitrile and water （0.1% formic acid）（85：15, v/v） as mobile phase in an isocratic mode of elution at a flow rate of 0.75 mL/min. MS detection was carried out in electrospray positive ion mode for the target ions and monitored at m/z 286.1465 for PPR and 272.1303 for the internal standard （IS）. The developed method exhibited a linear dynamic range over 0.01-2000 ng/mL for PPR on DBS. The overall extraction recovery of PPR from DBS was 92.5%. Influence of hematocrit and spot volume on DBS was also evaluated and found to be well within the acceptable limits. The method was successfully applied to pharmacokinetic studies of PPR in rats.

关键词： Dried blood spot LC-HRMS Piperine Pharmacokinetics Trichostachine

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Comparison of conventional and supported liquid extraction methods for the determination of sitagliptin and simvastatin in rat plasma by LC-ESI-MS/MS

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Journal of Pharmaceutical Analysis 2015年第3期5卷 161-168页

作者： B.Ramesh N.Manjula S.R.Bijargi V.U.M.Sarma P.sita devi Natural Products Chemistry Division Indian Institute of Chemical Technology Medicinal Chemistry & Pharmacology Division Indian Institute of Chemical Technology

Three extraction methods were compared for their efficiency to analyze sitagliptin and simvastatin in rat plasma by LC-MS/MS, including （1） liquid-liquid extraction （LLE）, （2） solid phase extraction （SPE） and （3） supported liquid extraction （SLE）. Comparison of recoveries of analytes with different extraction methods revealed that SLE was the best extraction method. The detection was facilitated with ion trap-mass spectrometer by multiple reactions monitoring （MRM） in a positive ion mode with ESI. The transitions monitored were m./z 441.1→325.2 for simvastatin, 408.2→235.1 for sitagliptin and 278.1→260.1 for the IS. The lower limit of quantification （LLOQ） was 0.2 ng/mL for sitagliptin and 0.1 ng/mL for simvastatin. The effective SLE offers enhanced chromatographic selectivity, thus facilitating the potential utility of the method for routine analysis of biological samples along with pharmacokinetic studies.

关键词： Rat plasma Simvastatin sita#'ptin Supported liquid extraction

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