Meister Isabel, Leonidova Anna, Kovač Jana, Duthaler Urs, Keiser Jennifer, Huwyler Jörg
Department of Medical Parasitology and Infection Biology, Swiss Tropical and Public Health Institute, Basel, Switzerland; University of Basel, P.O. Box, CH-4003 Basel, Switzerland.
Department of Medical Parasitology and Infection Biology, Swiss Tropical and Public Health Institute, Basel, Switzerland; University of Basel, P.O. Box, CH-4003 Basel, Switzerland.
J Pharm Biomed Anal. 2016 Jan 25;118:81-88. doi: 10.1016/j.jpba.2015.10.011. Epub 2015 Oct 22.
Praziquantel (PZQ) is the treatment of choice against various trematode and cestode infections. To study the pharmacokinetics of PZQ in patients infected with the liver fluke Opisthorchis viverrini, we developed and validated an enantioselective liquid chromatography coupled to tandem mass spectrometry method for the analysis of R - and S -PZQ and its R -trans-4-OH-PZQ metabolite in human plasma, blood and dried blood spots (DBS). The analytes were detected in the positive mode using selected reaction monitoring (R- and S-PZQ: m/z 312.2 → 202.2; R-trans -4-OH-PZQ: m/z 328.0 → 202.0). Prior to the chiral separation with a cellulose tris(3-chloro-4-methylphenylcarbamate) column, the analytes were purified from matrix contaminants and concentrated on a C-18 trapping column. The analytical range for each PZQ enantiomer was 0.01-2.5 μg/mL, and 0.1-25 μg/mL for the metabolite. The method met the requirements regarding precision (± 15%, ± 20% at the lower limit of quantification-LLOQ), intra- and inter-assay accuracy (85-115%, 80-120% at LLOQ), and linearity (R(2) ≥ 0.998). The analytes were stable in stock solutions as well as in plasma, blood and DBS. For DBS, the influences of hematocrit and blood spot size were considered as minor. Our validation results show that the method presented here is precise, accurate and selective, and can be used for pharmacokinetic studies. Moreover, the enantioselective separation was achieved with a run time of 11.5 min and a simple sample processing method.
吡喹酮(PZQ)是治疗各种吸虫和绦虫感染的首选药物。为了研究PZQ在感染肝吸虫华支睾吸虫患者体内的药代动力学,我们开发并验证了一种对映体选择性液相色谱-串联质谱法,用于分析人血浆、血液和干血斑(DBS)中的R-和S-PZQ及其R-反式-4-羟基-PZQ代谢物。使用选择反应监测在正模式下检测分析物(R-和S-PZQ:m/z 312.2 → 202.2;R-反式-4-羟基-PZQ:m/z 328.0 → 202.0)。在用三(3-氯-4-甲基苯基氨基甲酸酯)纤维素柱进行手性分离之前,将分析物从基质污染物中纯化出来,并在C-18捕集柱上进行浓缩。每种PZQ对映体的分析范围为0.01-2.5μg/mL,代谢物的分析范围为0.1-25μg/mL。该方法符合精密度(±15%,定量下限-LLOQ处为±20%)、批内和批间准确度(85-115%,LLOQ处为80-120%)以及线性(R(2)≥0.998)的要求。分析物在储备溶液以及血浆、血液和DBS中均稳定。对于DBS,血细胞比容和血斑大小的影响被认为较小。我们的验证结果表明,本文提出的方法精确、准确且具有选择性,可用于药代动力学研究。此外,采用11.5分钟的运行时间和简单的样品处理方法实现了对映体选择性分离。