液相色谱-串联质谱法测定养殖水体氯霉素残留量的研究  

Determination of Chloramphenicol Level in Aquaculture Water by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张秀妍 马琳 

机构地区：[1]大连市水产技术推广总站,辽宁大连116023

出　　处：《水生态学杂志》2015年第6期14-18,共5页Journal of Hydroecology

基　　金：辽宁省地方标准资助项目(2014333)

摘　　要：由于氯霉素对人体存在严重的毒副作用,是多个国家禁止使用的兽用药物,但在我国水产行业育苗、养殖和运输等环节仍然存在非法使用的情况,水产品药物残留例行监测中,氯霉素屡有检出,在水环境监测中,部分水域也检出了氯霉素,一些饭店暂养池中也检测出较高的氯霉素。实验水样取自养殖场、育苗室和饭店暂养池,选用乙酸乙酯为提取溶剂,液液萃取方式提取水中氯霉素,萃取时间3 min,应用液相色谱-串联质谱（LC-MS/MS）测定养殖水体中氯霉素的含量,量取250 m L水样,用100 m L乙酸乙酯分2次萃取,萃取液经旋转蒸发仪浓缩近干,以40%的甲醇-水溶液定容至1 m L。氯霉素标准系列溶液浓度为0.25、0.50、1.00、1.25、2.50、5.00 ng/m L,氘代氯霉素的含量均为2.0 ng/m L,上机检测,内标法定量。结果表明,氯霉素为外标,氘代氯霉素为内标,其峰面积比值（y）与浓度比值（x）的曲线方程为：y=1.136512x＋0.012050（R2=0.9990）;该方法氯霉素的检出限为2 ng/L,定量限为4 ng/L,仪器线性范围为0.25~5.00 ng/m L;加标浓度在2~20 ng/L时,平均回收率在80%~110%,相对标准偏差小于10%。应用证明该方法比较稳定、灵敏度高,适用于检测养殖水体中氯霉素的含量。Chloramphenicol is forbidden as a drug for veterinary use in China because of toxicity and serious side effects to humans. However,chloramphenicol is often determined in routine monitoring for drug residues in waterbased products,natural waters and even in the ponds of some restaurants. Thus,it is important to develop a reliable method for determining chloramphenicol in water to support monitoring,control sources of chloramphenicol and improve the detection index of pollution-free water. In this study,a high performance liquid chromatography-tandem mass spectrometric（ HPLC-MS / MS） method was developed to determine chloramphenicol levels in aquaculture water. Water samples were obtained from the aquafarm,seedling rearing rooms and storage ponds of restaurants. A250 m L water sample was extracted with 100 m L of ethyl acetate twice,each for three minutes and the extractant was concentrated to 1 m L prior to analysis. The analysis was carried out in the multi-reaction monitoring（ MRM）mode and the internal standard isotope dilution method was used for chloramphenicol quantification. The sensitivity and accuracy of the method was tested using a series of low concentration chloramphenicol standards（ 0. 25,0. 50,1. 00,1. 25,2. 50 and 5. 00 ng / m L）,all with cekafix as the internal standard at a concentration of 2. 0 ng / m L.The calibration curve for chloramphenicol exhibited good linearity over the concentration range from 0. 25 ng / m L to5. 0 ng / m L,with detection limit of 2 ng / L and quantification limit of 4 ng / L. When the standard addition concentration was in the range of 2- 20 ng / L,the average recovery rate was in the range of 80%- 110% and the relative standard deviation（ RSD） was less than 10%. The method proved to be accurate,stable and sensitive and meets the requirements for chloramphenicol detection in aquaculture water.

关 键 词：氯霉素 养殖水体 液相色谱-串联质谱法 

分 类 号：X502[环境科学与工程—环境工程]