Wang Xianqin, Xiang Zheng, Cai Xiaojun, Wu Haiya, Wang Xuebao, Li Junwei, Zhang Meiling
Analytical and Testing Center, Wenzhou Medical College, Wenzhou 325035, China.
Biomed Chromatogr. 2011 Jul;25(7):833-7. doi: 10.1002/bmc.1524. Epub 2010 Sep 27.
A sensitive and selective liquid chromatography-tandem mass spectrometry method for the determination of pethidine in human plasma was developed and validated over the concentration range of 4-2000 ng/mL. After addition of ketamine as internal standard, liquid-liquid extraction was used to produce a protein-free extract. Chromatographic separation was achieved on a 100 × 2.1 mm, 5 µm particle, Allure™ PFP propyl column, with 45:40:15 (v/v/v) acetonitrile-methanol-water containing 0.2% formic acid as mobile phase. The MS data acquisition was accomplished by multiple reactions monitoring mode with positive electrospray ionization interface. The lower limit of quantification was 4 ng/mL; for inter-day and intra-day tests, the precision (RSD) for the entire validation was less than 7%, and the accuracy was within 95.9-106.5%. The method is sensitive and simple, and was successfully applied to analysis of samples of clinical intoxication.
建立了一种灵敏且具选择性的液相色谱-串联质谱法，用于测定人血浆中的哌替啶，该方法在4 - 2000 ng/mL浓度范围内得到验证。加入氯胺酮作为内标后，采用液-液萃取法制备无蛋白提取物。在100×2.1 mm、5 µm粒径的Allure™ PFP丙基柱上进行色谱分离，以45:40:15（v/v/v）含0.2%甲酸的乙腈-甲醇-水为流动相。通过带正电喷雾电离接口的多反应监测模式完成质谱数据采集。定量下限为4 ng/mL；日间和日内试验中，整个验证过程的精密度（相对标准偏差）小于7%，准确度在95.9 - 106.5%范围内。该方法灵敏且简便，已成功应用于临床中毒样本的分析。
