液相质谱联用法测定淡水鱼及鸡蛋中氯霉素类化合物残留  

Detection of Chloramphenicol Compounds Vestigital in Fish and Egg by UHPLC-MS/MS

作　　者：田卫政 TIAN Weizheng(Shanghai Chongming Institutes for Food and Drug Control,Shanghai 202150)

机构地区：[1]上海市崇明食品药品检验所/崇明区食品安全检测中心,崇明202150

出　　处：《食品工业》2024年第9期316-320,共5页The Food Industry

摘　　要：建立一种同时测定鱼肉及蛋类中氯霉素、甲砜霉素、氟苯尼考及其代谢物氟苯尼考胺的超高效液相串联质谱法。样品中加入氯霉素-D5内标,用2%氨化乙酸乙酯提取离心后,用正己烷和水进行液液萃取提取目标化合物后上机分析。仪器条件,采用甲醇-0.1%乙酸铵水溶液(40+60,V/V)为流动相进行等度洗脱,过ZORBAX Eclipse Plus C_(18)色谱柱(1.8μm,3.0 cm×50 mm),ESI电离源正/负离子模式切换多反应监测采集离子对数据,采用内标法对氯霉素、甲砜霉素、氟苯尼考及氟苯尼考胺进行定量。氯霉素、甲砜霉素、氟苯尼考在0.1~1μg/L质量浓度范围内具有良好线性关系,相关系数r>0.995;氟苯尼考胺在0.5~5μg/L质量浓度范围内具有良好线性关系,相关系数r>0.999。考察淡水鱼和鸡蛋2个基质,在0.1,0.2和1.0μg/kg加标水平下,氯霉素、甲砜霉素、氟苯尼考的平均回收率在80.8%~107.2%之间,相对标准偏差S_(RSD)为1.3%~8.6%。氟苯尼考胺在0.5,1.0和5.0μg/kg加标水平下,回收率在90.8%~102.1%之间,相对标准偏差SRSD为1.6%~6.2%(n=6)。氯霉素、甲砜霉素、氟苯尼考的检出限为0.02μg/kg,氟苯尼考胺的检出限为0.1μg/kg。该方法操作简单、准确性、灵敏度、稳定性良好,适用于进行淡水鱼及鸡蛋品中氯霉素类化合物的检测。A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was developed for detection 4 chloramphenicol residues including chloramphenicol,thiamphenicol,florfenicol and florfenicol amine in fish and egg.Samples were extracted with 2%ammonia ethyl acetate solution with chromatography-D5.The mobile phase was composed of methanol and 0.1%ammonium acetate solution.ZORBAX Eclipse Plus C_(18)(1.8μm,3.0 cm×50 mm)was selected as chromatographic column.Monitoring was conducted in electrospray positive/negative ion switching multireaction mode(MRM).Isotope internal standard method was used for chloramphenicol,thiamphenicol,florfenicol and florfenicol amine detection.Chloramphenicol,thiamphenicol and florfenicol showed good linearity in the range of 0.1-1μg/L,and the correlation coefficients were greater than 0.995.Florfenicol amine showed good linearity in the range of 0.5-5μg/L,and the correlation coefficients were greater than 0.999.The recovery rates of chloramphenicol,thiamphenicol,florfenicol in fish and egg samples at spiked levels of 0.1,0.2 and 1.0μg/kg were between 80.8%and 107.2%with the S_(RSD) range from 1.3%to 8.6%(n=6).The recovery rates of florfenicol amine in fish and egg samples at spiked levels of 0.5,1.0 and 5.0μg/kg were between 90.8%and 102.1%with the SRSD range from 1.6%to 6.2%(n=6).The limit of detection of chloramphenicol,thiamphenicol and florfenicol was 0.02μg/kg,and the limit of florfenicol amine was 0.1μg/kg.The method is simple to operate with high sensitivity and accuracy.It can be applied to detect chloramphenicol,thiamphenicol,florfenicol and florfenicol amine in fish and eggs.

关 键 词：超高效液相色谱-串联质谱法 鸡蛋 淡水鱼 氯霉素 甲砜霉素 氟苯尼考 氟苯尼考胺 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学] TS253.7[轻工技术与工程—水产品加工及贮藏工程]