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 C18色谱柱(1.8 µm,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0.1～1 μg/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0.5～5 μg/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1.0 μg/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SRSD为1.3％～8.6％.氟苯尼考胺在0.5,1.0和5.0 µg/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)o氯霉素、甲砜霉素、氟苯尼考的检出限为0.02 μg/kg,氟苯尼考胺的检出限为0.1 μg/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.
Detection of Chloramphenicol Compounds Vestigital in Fish and Egg by UHPLC-MS/MS
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 C18(1.8 μm,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 0.1-1 μg/L,and the correlation coefficients were greater than 0.995.Florfenicol amine showed good linearity in the range of 0.5-5 μg/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 1.0 μg/kg were between 80.8％and 107.2％with the SRSD 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 5.0 μg/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 0.02 μg/kg,and the limit of florfenicol amine was 0.1 μg/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.
万方数据
维普
