超高效液相色谱串联质谱法检测血液中的氨曲南及甲硝唑

发布时间：2018-09-09 11:52

【摘要】：目的建立同时检测血液中氨曲南及甲硝唑的超高效液相色谱串联质谱分析方法。方法以头孢拉定和氯霉素为内标,血液样品经乙腈沉淀蛋白后通过高效液相色谱分离,电喷雾离子源进行离子化,采用多反应监测方式(multiple reaction monitoring mode,MRM)对各化合物进行监测。结果所建立的方法可同时检测血液中的氨曲南和甲硝唑成分,氨曲南在10~5 000 ng/mL、甲硝唑在1~1 000 ng/mL的线性范围内具有良好的线性关系,线性相关系数r均大于0.995;血液中氨曲南和甲硝唑的检出限分别为5和0.5 ng/mL(S/N=3∶1);定量限分别为10和1 ng/mL(S/N=10∶1);方法的日间及日内精密度均小于10%,准确度为89.6%~97.5%。将此方法应用于1例医疗纠纷案件的鉴定,在涉案死者的血液中同时检出氨曲南及甲硝唑成分,血液中氨曲南及甲硝唑的质量浓度分别为438 ng/mL和15μg/mL。结论本研究所建立的分析方法灵敏度高、简便快速、专属性强、可靠性高,为司法鉴定实践中涉及氨曲南和甲硝唑的案件提供了技术支持和基础数据。
[Abstract]:OBJECTIVE To establish a method for simultaneous determination of aztreonam and metronidazole in blood by ultra-high performance liquid chromatography tandem mass spectrometry.METHODS Cefradine and chloramphenicol were used as internal standard,protein was precipitated by acetonitrile and separated by high performance liquid chromatography,ionized by electrospray ionization,and multi-reaction monitoring was used. Results The established method could simultaneously detect aztreonam and metronidazole in blood. The linear relationship between aztreonam and metronidazole was good in the linear range of 10-5 000 ng/mL, 1-1 000 ng/mL, and the linear correlation coefficient r was greater than 0.995. The quantitative limits were 10 ng/mL and 1 ng/mL (S/N=10:1), respectively, and the intra-day and intra-day precision were less than 10% and 89.6% ~ 97.5% respectively. CONCLUSION The method is sensitive, simple, rapid, specific and reliable. It provides technical support and basic data for the cases involving aztreonam and metronidazole in forensic practice.
【作者单位】： 司法部司法鉴定科学技术研究所上海市法医学重点实验室上海市司法鉴定专业技术服务平台;
【基金】：十三五国家重点研发计划项目(2016YFC0800700-4) 国家自然科学基金青年项目(81501633) 上海市法医学重点实验室项目(17DZ2273200) 上海市司法鉴定专业技术服务平台资助项目(16DZ2290900)~~
【分类号】：D919
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