超高效液相色谱-串联质谱法同时测定人血清中甲硝唑和氯霉素  

Analysis of metronidazole and chloramphenicol in human serum by ultra performance liquid chromatography tandem mass spectrometry

作　　者：曹杰[1] 王强[2] 郝世轩 宋寅生[1] 和佳鸳 徐虹[1] CAO Jie;WANG Qiang;HAO Shi-xuan;SONG Yin-sheng;HE Jia-yuan;XU Hong(Zhenjiang Municipal Center for Disease Control and Prevention,Jiangsu 212004,China;不详)

机构地区：[1]镇江市疾病预防控制中心,江苏212004 [2]江苏大学医学院

出　　处：《中国卫生检验杂志》2023年第5期528-531,共4页Chinese Journal of Health Laboratory Technology

基　　金：2020年度镇江市科技创新资金(重点研发计划—社会发展)项目(SH2020039)。

摘　　要：目的 建立同时测定人血清中甲硝唑和氯霉素的超高效液相色谱-串联质谱法。方法 血清样品经乙腈沉淀、离心、过滤后进样,以甲醇-0.05%氨水溶液为流动相进行梯度洗脱,采用Waters BEH C18色谱柱(2.1 mm×100 mm, 1.7μm)分离,在电喷雾离子源、多反应监测模式下检测,同位素内标法定量。结果 在2.20 ng/ml~1 100 ng/ml浓度内,甲硝唑和氯霉素线性关系良好,相关系数均>0.998,方法检出限为0.55 ng/ml,平均回收率为94.0%~109.0%,相对标准偏差为2.3%~9.2%。血清样品中待测物的短期、长期和冻融稳定性良好。样品基质对氯霉素的基质效应可忽略,而对甲硝唑具有基质抑制作用。结论 该方法操作简便、快速、灵敏度高、准确性好,符合生物样品测定的技术要求,适用于同时测定人血清中甲硝唑和氯霉素。Objective This paper aims to establish an ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method for the determination of metronidazole and chloramphenicol in human serum. Methods The serum samples were precipitated with acetonitrile, centrifuged and then filtrated, and finally separated by a Waters BEH C18column(2.1 mm×100 mm, 1.7 μm). Methanol-0.05% ammonia aqueous solution was used as mobile phase. The detection was performed under multiple reaction monitoring mode. The quantification was based on internal standard curves. Results The linear relationship of metronidazole and chloramphenicol were within 2.20 ng/ml-1 100 ng/ml, with the linear correlation coefficient greater than 0.998. The limit of detection(LODs) were all 0.55 ng/ml, and the average recoveries of low, medium and high spiked levels were within 94.0%-109.0%, with the relative standard deviations(RSDs) of 2.3%-9.2%. Metronidazole and chloramphenicol in serum samples were stable for short-term, long-term, and freeze-thaw. Chloramphenicol was not interfered by matrix effect, but metronidazole was inhibited by the matrix effect. Conclusion The method is fast, simple, sensitive and accurate, which meets the technical determination requirements of biological samples and is suitable for the determination of metronidazole and chloramphenicol in human serum.

关 键 词：超高效液相色谱-串联质谱法 甲硝唑 氯霉素 血清 

分 类 号：O657.63[理学—分析化学]