摘要
研究创建固相萃取-液质色谱-质谱法检测水产养殖水中的孔雀石绿及其代谢物、氧氟沙星、恩诺沙星和土霉素微量残留的分析方法。随机在水产养殖厂采集水产养殖水样2 L,过滤以去除肉眼可见异物,加0.1 mol/L氢氧化钠或盐酸溶液,调节pH值至7.0,取预处理过的水样1 L置样品架上,以15 mL/min的流量,过固相萃取柱,最后用15 mL 50%甲醇洗脱,收集洗脱液,最后将洗脱液于水浴45℃氮吹至近干,再加甲醇定容至1 mL,混匀,上液相色谱-质谱仪定量检测。孔雀石绿、隐色孔雀石绿、氧氟沙星、恩诺沙星和土霉素在0.002~4.0μg/mL浓度范围内,线性系数均大于0.995,线性关系良好;5种目标物检出限范围在0.07~0.47μg/mL之间;平均回收率在87.2%~102.6%之间;重复性相对标准偏差在5.0%以内。结果证明,此方法检出限低、操作步骤简单、检测结果准确,适用于水产养殖水中极微量杀菌剂、抗生素等残留的检测。
To establish a method for the determination of malachite green and its metabolites,ofloxacin,enrofloxacin and oxytetracycline in aquaculture water by solid phase extraction using liquid chromatography mass spectrometry.2 litre of aquaculture water samples were collected randomly in the aquaculture plant,filtered to remove the visible foreign bodies,added 0.1 mol/L sodium hydroxide or hydrochloric acid solution,adjusted the pH value to 7.0,took 1 litre of pretreated water sample on the sample rack,passed through the solid phase extraction column at the flow rate of 15 mL/min,finally eluted with 15 mL 50%methanol,collected the eluent,and finally put the eluent in the water bath at 45℃.Then add methanol to 1 mL,mixed well,and conduct quantitative detection by HPLC-MS.The linear range of malachite green,leucomalachite green,ofloxacin,enrofloxacin and oxytetracycline was from 0.002 to 4.0μg/mL,the linear coefficients were greater than 0.995,the linear relationship was good;the detection limits of the five targets were 0.07-0.47μg/mL;the average recoveries were 87.2%-102.6%;the relative standard deviation of repeatability was less than 5.0%.The experimental results showed that this method had the advantages of low detection limit,simple operation steps and accurate detection results,which was suitable for the detection of extremely trace fungicides,antibiotics and other residues in aquaculture water.
作者
郭伟伟
孙志洪
GUO Weiwei;SUN Zhihong(Cangzhou Ecological Environment Monitoring Center,Cangzhou 061000,China;Cangzhou Ecological Environment Monitoring Center of Hebei Province,Cangzhou 061000,China)
出处
《中国测试》
CAS
北大核心
2022年第1期80-84,共5页
China Measurement & Test
关键词
固相萃取
液相色谱-质谱法
水产养殖水
孔雀石绿
土霉素
solid phase extraction
liquid chromatography-mass spectrometry
aquaculture water
malachite green
oxytetracycline
作者简介
郭伟伟(1982-),男,河北沧州市人,高级工程师,主要从事环境监测和科研工作;通讯作者:孙志洪(1983-),男,河北沧州市人,高级工程师,主要从事环境监测等工作。
