[1]陈顺琴,高焕,朱发泽,等.超高效液相色谱 -串联质谱测定污水中依托咪酯[J].中国给水排水,2024,40(4):132-136.
　CHENShun-qin,GAOHuan,ZHUFa-ze,et al.Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry for Determination of Etomidate in Wastewater[J].China Water & Wastewater,2024,40(4):132-136.
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超高效液相色谱 -串联质谱测定污水中依托咪酯

中国给水排水[ISSN:1000-4062/CN:12-1073/TU] 卷: 第40卷 期数: 2024年第4期 页码: 132-136 栏目: 出版日期: 2024-02-17
Title:
Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry for Determination of Etomidate in Wastewater
作者:
陈顺琴1， 高焕1， 朱发泽1， 陈月猛2， 刘杉2， 丁文波3， 刘玉波1
（1.贵州医科大学 法医学院，贵州 贵阳 550004；2.贵阳市公安局 毒品检验中心，贵州 贵阳 550018；3.贵州万孚先义检测技术有限公司，贵州 贵阳 550009）
Author(s):
CHEN　Shun-qin1， GAO　Huan1， ZHU　Fa-ze1， CHEN　Yue-meng2， LIU Shan2， DING　Wen-bo3， LIU　Yu-bo1
（1. School of Forensic Medicine， Guizhou Medical University， Guiyang 550004， China； 2. Drug Identification Center， Guiyang Municipal Public Security Bureau， Guiyang 550018， China； 3. Guizhou Wanfu Xianyi Testing Technology Limited Company， Guiyang 550009， China）
关键词:
超高效液相色谱-串联质谱(UPLC-MS/MS);  依托咪酯;  污水
Keywords:
UPLC-MS/MS;  etomidate;  wastewater
摘要:
基于超高效液相色谱-串联质谱（UPLC-MS/MS）技术首次建立了污水中依托咪酯的分析检测方法，样品经在线固相萃取（On?line SPE）系统，以HLB Direct Connect HP固相萃取小柱（2.1 mm×30 mm，20 μm）对目标化合物进行萃取后，采用乙腈-2 mmol/L甲酸铵和0.1%甲酸水溶液为流动相进行梯度洗脱，再将目标物反向加载至Kinetex Biphenyl色谱柱（3.0 mm×100 mm，2.6 μm），采用电喷雾正离子（ESI+）、多反应监测（MRM）模式分析检测。结果显示，依托咪酯在1～300 ng/L范围内线性关系良好，R2为0.999 7，方法检出限（LOD）为0.3 ng/L，定量限（LOQ）为1.0 ng/L。应用该方法对遵义地区17座污水处理厂进水口处依托咪酯的浓度进行检测，进一步验证了该方法的可靠性。污水样品中依托咪酯的检出率较低，其原因可能是依托咪酯经体内代谢后主要以依托咪酯酸的形式存在，检测结果与实际情况相符。依托咪酯于2023年10月1日起被纳入第二类精神药品列管目录，该方法的建立对依托咪酯的分析提供了技术参考。
Abstract:
This paper established a method for analyzing and detecting etomidate in wastewater for the first time based on ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The target compounds in the wastewater samples were extracted by on-line solid phase extraction (on-line SPE) system with HLB Direct Connect HP solid phase extraction column (2.1 mm×30 mm, 20 μm). Then, acetonitrile, 2 mmol/L ammonium formate and 0.1% formic acid aqueous solution were employed as mobile phase for gradient elution, and the target compounds were reverse loaded to Kinetex Biphenyl column (3.0 mm×100 mm; 2.6 μm) and eventually analyzed by using electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode analysis. Etomidate had a good linear relationship in the range of 1-300 ng/L. The R2 was 0.999 7, the limit of detection (LOD) was 0.3 ng/L, and the limit of quantitation (LOQ) was 1.0 ng/L. The method was applied to detect the concentration of etomidate in the inlet of 17 wastewater treatment plants in Zunyi, and the reliability of the method was further verified. The low detection rate of etomidate in wastewater samples might be due to the fact that etomidate existed mainly in the form of etomidate acid after metabolism in body, and the detection results were consistent with the actual situation. Etomidate has been included in the second category of psychotropic drugs since October 1, 2023, and the establishment of this method provides a technical reference for the detection of etomidate.
更新日期/Last Update: 2024-02-17