摘要
建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定蜂蜜中氯霉素、硝基咪唑类及其代谢物残留量的分析方法。实验对样品前处理过程及色谱质谱仪器条件进行优化。蜂蜜样品与超纯水1∶1混合后涡旋振荡溶解,经乙腈溶液超声提取,再加入氯化钠盐析分层,离心后上清液采用C18和PSA吸附剂进行净化处理,以ACQUITY BEH C18色谱柱分离。在电喷雾离子(electrospray ionization,ESI)源正、负离子切换扫描模式下,采用多反应监测(multiple reaction monitoring,MRM)模式进行检测,外标法进行定量。结果表明,8种目标化合物在3 min内实现良好分离,在0.1~50μg/L质量浓度范围内呈现良好线性关系,相关系数(R2)均大于0.998,其中氯霉素的检出限(limit of detection,LOD)、定量限(limit of quantification,LOQ)分别为0.09μg/kg和0.20μg/kg,7种硝基咪唑类药物的LODs和LOQs分别为0.50~1.50μg/kg和1.50~3.00μg/kg。在低、中、高3个浓度添加水平下的加标回收率为81.2%~95.5%,相对标准偏差(relative standard deviations,RSDs)为1.2%~4.2%(n=6)。该方法稳定、准确、灵敏、快速,适用于蜂蜜中氯霉素和硝基咪唑类药物的快速检测和分析确证。
To establish a method for simultaneous determination of chloramphenicol,nitroimidazoles and metabolites in honey by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The pretreatment process and instrument conditions were optimized.Samples were mixed with ultrapure water at a ratio of 1:1,ultrasonic extracted with acetonitrile solution and salted out by adding NaCl.After centrifugation,the supernatant was cleaned up by C18 and PSA,and separated on an ACQUITY BEH C18 column.In the electrospray ionization(ESI)positive and negative ion switching scanning mode,the samples were analyzed by multiple reaction monitoring(MRM)and quantified by external standard method.Result showed that all the 8 target compounds were well separated in 3 min and the calibration curves in the range of 0.1-50μg/L for all compounds were linear with correlation coefficients(R2)were more than 0.998.The limit of detection(LOD)and limit of quantification(LOQ)for chloramphenicol were 0.09μg/kg and 0.20μg/kg,respectively.For 7 nitroimidazoles,the LODs and LOQs were 0.50-1.50μg/kg and 1.50-3.00μg/kg,respectively.The average recoveries at low,medium and high spiked levels were ranged from 81.2%-95.5%,with relative standard deviations(RSDs)in the range of 1.2%-4.2%(n=6).The method is proved to be stable,accurate,sensitive and rapid,and can meet requirements for the rapid and accurate determination of chloramphenicol and nitroimidazoles in honey.
作者
倪杨
杨军军
石磊
张莹莹
熊融
Ni Yang;Yang Junjun;Shi Lei;Zhang Yingying;Xiong Rong(Institute of Forestry and Pomology,Beijing Academy of Agriculture and Forestry Sciences,Beijing Engineering Research Center for Deciduous Fruit Trees,Inspection and Testing Laboratory of Fruits and Nursery Stocks(Beijing)Ministry of Agriculture and Rural Affairs,Beijing 100093,China)
出处
《中国蜂业》
2022年第8期56-60,共5页
Apiculture of China
基金
北京市科技计划项目(Z201100008920007)
北京市农林科学院科技创新能力建设专项(KJCX20200302)。
