Bharathi D Vijaya, Hotha Kishore Kumar, Jagadeesh B, Chatki Pankaj K, Thriveni K, Mullangi Ramesh, Naidu A
Bioanalytical Department, Integrated Product Development, Dr Reddy's Laboratories Ltd, Bachupalli, Hyderabad-500 072, India.
Biomed Chromatogr. 2009 Jul;23(7):732-9. doi: 10.1002/bmc.1177.
A highly selective, sensitive and accurate HPLC method has been developed and validated for the estimation of four proton-pump inhibitors (PPI), lansoprazole (LPZ), omeprazole (OPZ), pantoprazole (PPZ) and rabeprazole (RPZ), with 500 microL human plasma using zonisamide as an internal standard (IS). The sample preparation involved simple liquid-liquid extraction of LPZ, OPZ, PPZ and RPZ and IS from human plasma with ethyl acetate. The baseline separation of all the peaks was achieved with 0.1% triethylamine (pH 6.0):acetonitrile (72:28, v/v) at a flow rate of 1 mL/min on a Zorbax C(8) column. The total chromatographic run time was 11.0 min and the simultaneous elution of IS, OPZ, RPZ, PPZ and LPZ occurred at approximately 2.42, 4.45, 5.02 and 9.37 min, respectively. The method was proved to be accurate and precise at linearity range of 20.61-1999.79 ng/mL with a correlation coefficient (r) of >or=0.999. The limit of quantitation for each of the PPI studied was 20.61 ng/mL. The intra- and inter-day precision and accuracy values were found to be within the assay variability limits as per the FDA guidelines. The developed assay method was applied to a pharmacokinetic study in human volunteers.
已开发并验证了一种高选择性、灵敏且准确的高效液相色谱法，用于测定四种质子泵抑制剂（PPI），即兰索拉唑（LPZ）、奥美拉唑（OPZ）、泮托拉唑（PPZ）和雷贝拉唑（RPZ），以内标（IS）唑尼沙胺为内标，使用500微升人血浆。样品制备包括用乙酸乙酯从人血浆中简单液液萃取LPZ、OPZ、PPZ、RPZ和IS。在Zorbax C(8)柱上，以0.1%三乙胺（pH 6.0）：乙腈（72:28，v/v）为流动相，流速为1 mL/min，实现了所有峰的基线分离。总色谱运行时间为11.0分钟，IS、OPZ、RPZ、PPZ和LPZ的同时洗脱分别出现在约2.42、4.45、5.02和9.37分钟。该方法在20.61 - 1999.79 ng/mL的线性范围内被证明准确且精密，相关系数（r）≥0.999。所研究的每种PPI的定量限为20.61 ng/mL。根据FDA指南，日内和日间精密度及准确度值均在分析变异性限度内。所开发的分析方法应用于人体志愿者的药代动力学研究。
