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目的:建立超高效液相色谱-质谱法(UPLC-MS/MS法)测定人血液、肝脏中维库溴铵。方法:取空白血、空白肝(经匀浆)加入一定量维库溴铵标准溶液,加入pH 8氨水稀释后涡旋离心,取上清液过混合型弱阳离子交换柱(WCX)进行固相萃取提取纯化。提取液采用UPLC-MS/MS检测。色谱分离采用UPLC~?BEH HILIC色谱柱。流动相体系:A相为乙腈,B相为5 mmol·L~(-1)甲酸铵水溶液(甲酸调pH 3.5左右),梯度淋洗;质谱检测采用正离子扫描,多反应离子监测模式(MRM)。检测结果以维库溴铵母离子m/z 557.526和子离子m/z 100.103、356.346进行定性、定量。结果:空白血、空白肝加标回收率在74%~120%,检出限为0.43 ng·mL~(-1)。结论:本文通过初步探讨维库溴铵大鼠体内分布,得知维库溴铵在大鼠体内的分布变化是受多种复杂因素影响的动态变化过程,并且死后随提取检材部位的不同测出药物浓度存在较大差异。真实案例中也证实了维库溴铵体内分布这一特点。本文可以为相关中毒案(事)件的检验提供方法,并且满足检验要求。
Objective: To establish a method for the determination of vecuronium in human blood and liver by ultra performance liquid chromatography-mass spectrometry (UPLC-MS / MS). Methods: Blank blood and blank liver (homogenized) were added into a certain amount of vecuronium standard solution, diluted with pH 8 ammonia solution and vortexed for centrifugation. The supernatant was mixed with weak cation exchange column (WCX) Extraction and purification. The extract was detected by UPLC-MS / MS. Chromatography using UPLC ~? BEH HILIC column. The mobile phase consisted of phase A acetonitrile and phase B 5 mmol·L -1 ammonium formate (adjusted to pH 3.5 with formic acid) and gradient elution. The mass spectrometry was performed with positive ion scan and multi-reactive ion monitoring (MRM) ). The test results were qualitative and quantitative with veccuronium ion m / z 557.526 and ion m / z 100.103,356.346. Results: The spiked recoveries of blank and blank liver ranged from 74% to 120% with a detection limit of 0.43 ng · mL -1. CONCLUSIONS: In this study, we first investigated the distribution of vecuronium in rats and found that the change of vecuronium in rats is a dynamic process influenced by many complicated factors. Measured drug concentration there is a big difference. The real case also confirmed the in vivo distribution of vecuronium. This article can provide methods for the inspection of poisoning cases, and to meet inspection requirements.