高效液相色谱-串联质谱法测定池塘沉积物中氯霉素残留  

Determination of chloramphenicol residue in pond sediment by UPLC-MS/MS

作　　者：张素青[1] 陈永平[1] 李春青[1] 高丽娜[1] 李连庆[1] 时文博[1] 李兆千[1] 张丹娜[1] 

机构地区：[1]农业部渔业环境及水产品质量监督检验测试中心(天津),天津300221

出　　处：《中国渔业质量与标准》2017年第4期14-20,共7页Chinese Fishery Quality and Standards

基　　金：天津市科技支撑计划重点项目(14ZCZDNC00012)

摘　　要：[目的]建立一种使用液相色谱-串联质谱联用仪快速准确检测池塘沉积物中痕量氯霉素残留的方法,为水产品中氯霉素污染来源的排查提供技术支持。[方法]底泥经润湿后,经乙酸乙酯水饱和溶液提取,Sep-Pa K C_(18)固相萃取柱净化,Shim-Pack XR-ODS色谱柱分离,采用甲醇和水为流动相,并用梯度洗脱对待测物进行分离,以氘代氯霉素(氯霉素-D5)为内标,采用负离子扫描,多反应监测模式(MRM),定性离子对m/z为321→152.0,256.8,定量离子对m/z为321→152.0。[结果]氯霉素类药物在0.5~10.0 ng/m L范围内线性良好,相关系数均大于0.99,本方法的检出限为0.1μg/kg,定量限为0.3μg/kg。3个加标水平(0.5、1.0和5.0μg/kg)的平均回收率为90.1%~96.6%,相对标准偏差为2.4%~7.0%。[结论]实验结果符合氯霉素药物残留检测的相关法规要求,适用于淡水池塘沉积物中氯霉素残留的定性定量检测。[Objectives]This study is aim to establish a rapid and accurate method for trace analysis of chloramphenicol residue in pond sediment. It will provide methodological guidance for investigating chloramphenicol pollution in aquatic products. [Methods] The mud samples were soaked and extracted using water saturated ethyl acetate solution by liquid-liquid extraction method. After extraction,the samples were purified by Sep-Pak C_（18） and separated by Shim-Pack XR-ODS columns with a mobile phase of methanol and water using gradient elution. Chloramphenicol-D5 was used as internal reference standard and multiple reaction monitoring combined with negative-ion scans was performed. Characteristic transition reaction fragments m/z： 321→152. 0,256. 8 and m/z： 321→152. 0 were tested for the qualitative ion pair and quantitative ion pair of chloramphenicol,respectively. [Results] The dosage of chloramphenicol residues（ 0. 5 ~ 10. 0 ng/m L） fit well on the calibration curve of CPS intensity. The correlation coefficient was above 0. 99. The limit of detection and quantification for chloramphenicol were 0. 1 μg/kg and 0. 3 μg/kg,respectively. The average recoveries of chloramphenicol at the levels of 0. 5,1. 0,and 5. 0 μg/kg were ranged from90. 1% to 96. 6%. The relative standard deviation was 2. 4% ~ 7. 0%. [Conclusions]The test results confirmed totally to the requirements of related regulation and this method is suitable for the qualitative and quantitative detection of chloramphenicol residues in pond sediment.

关 键 词：高效液相色谱-串联质谱 池塘沉积物 氯霉素 残留量 

分 类 号：O657.63[理学—分析化学] S948[理学—化学]