Chi Jingduan, Jayewardene Anura L, Stone Judith A, Motoya Toshiro, Aweeka Francesca T
Department of Clinical Pharmacy, Drug Research Unit, School of Pharmacy, University of California, San Francisco, CA 94143, USA.
J Pharm Biomed Anal. 2002 Oct 15;30(3):675-84. doi: 10.1016/s0731-7085(02)00357-6.
A sensitive and rapid liquid chromatography tandem mass spectrometry (LC-MS-MS) method has been developed to measure the levels of five HIV protease inhibitors nelfinavir (NFV), indinavir (IDV), ritonavir (RTV), saquinavir (SQV) and amprenavir (APV) in human plasma. The analytes and internal standard are isolated from plasma by a simple acetonitrile precipitation of plasma proteins followed by centrifugation. LC-MS-MS in positive mode used pairs of ions at m/z of 568.4/330.0, 614.3/421.2, 720.9/296.0, 671.1/570.2 and 505.9/245.0 for NFV, IDV, RTV, SQV and APV, respectively and 628/421 for the internal standard. Two 1/x weighted linear calibration curves for each analyte were established for quantitation with the low curve ranging from 5 to 1000 ng/ml and while the high curve ranging from 1000 to 10,000 ng/ml. Mean inter- and intra-assay coefficients of variation (CVs) over the ranges of the standard curves were less than 10%. The overall recovery of NFV, IDV, RTV, SQV and APV were 88.4, 91.4, 92.2, 88.9 and 87.6%, respectively.
已开发出一种灵敏且快速的液相色谱串联质谱法（LC-MS-MS）来测定人血浆中五种HIV蛋白酶抑制剂的水平，这五种抑制剂分别是奈非那韦（NFV）、茚地那韦（IDV）、利托那韦（RTV）、沙奎那韦（SQV）和安普那韦（APV）。通过用乙腈简单沉淀血浆蛋白然后离心，从血浆中分离出分析物和内标。正模式下的LC-MS-MS分别使用m/z为568.4/330.0、614.3/421.2、720.9/296.0、671.1/570.2和505.9/245.0的离子对来测定NFV、IDV、RTV、SQV和APV，使用628/421的离子对来测定内标。为每种分析物建立了两条1/x加权线性校准曲线用于定量，低曲线范围为5至1000 ng/ml，高曲线范围为1000至10,000 ng/ml。标准曲线范围内的平均批间和批内变异系数（CVs）均小于10%。NFV、IDV、RTV、SQV和APV的总体回收率分别为88.4%、91.4%、92.2%、88.9%和87.6%。
