同位素稀释高效液相色谱-串联质谱法测定水体、底泥、鱼及虾中氯硝柳胺残留量  

Determination of Niclosamide in Water,Sediment,Fish and Shrimp by HPLC-MS/MS Method with Isotope Dilution

作　　者：刘永涛[1,2,3] 沈丹怡 董靖[1,3] 杨秋红[1,3] 杨移斌 周顺[1,3] 艾晓辉 LIU Yong-tao;SHEN Dan-yi;DONG Jing;YANG Qiu-hong;YANG Yi-bin;ZHOU Shun;AI Xiao-hui(Yangtze River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Wuhan 430223,China;Key Laboratory of Control of Quality and Safety for Aquatic Products,Ministry of Agriculture and Rural Affairs,Beijing 100141,China;Hubei Province Engineering and Technology Research Center of Aquatic Product Quality and Safety,Wuhan 430223,China;Spreading Center of Technology in Aquatic Science of Cixi City in Zhejiang Province,Cixi 315300,China)

机构地区：[1]中国水产科学研究院长江水产研究所,湖北武汉430223 [2]农业农村部水产品质量安全控制重点实验室,北京100141 [3]湖北省水产品质量安全工程技术研究中心,湖北武汉430223 [4]浙江省慈溪市水产技术推广中心,浙江慈溪315300

出　　处：《分析测试学报》2020年第8期980-985,共6页Journal of Instrumental Analysis

基　　金：国家重点研发计划课题(2019YFD0901701);现代农业人才支撑计划项目(2016-2020)。

摘　　要：建立了水体、底泥、鱼体自然比例带皮肌肉和虾肌肉中氯硝柳胺(NIC)残留量测定的同位素稀释高效液相色谱-串联质谱(HPLC-MS/MS)法。水样经碱化后以乙酸乙酯提取,其他样品采用0.1%氨水乙腈提取,C18粉进行样品净化。以乙腈-水为流动相,流速为0.3 mL/min,采用Thermo Hypersil Gold C18(150 mm×2.1 mm,5μm)色谱柱进行分离,氯硝柳胺稳定同位素标记物(氯硝柳胺-13C6)为内标,选择反应监测(SRM)模式扫描,内标法定量。结果表明氯硝柳胺在0.2~200μg/L范围内呈良好线性关系,相关系数(r2)不小于0.9995。空白水样在2.5、25、250 ng/L加标水平下的平均回收率为90.5%~109%,相对标准偏差(RSD)为3.2%~11%,检出限(LOD)为1.0 ng/L,定量下限(LOQ)为2.5 ng/L;空白底泥、黄颡鱼自然比例带皮肌肉和克氏原螯虾肌肉在0.5、5.0、50μg/kg加标水平下的平均回收率分别为89.4%~113%、92.8%~110%和94.1%~107%,RSD分别为4.6%~12%、2.8%~11%和3.2%~9.3%,LOD均为0.2μg/kg,LOQ均为0.5μg/kg。该方法的灵敏度、准确度和选择性高,适用于实际水产养殖环境水体、底泥、鱼和虾中氯硝柳胺的残留分析。A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) with isotope dilution was established for the determination of niclosamide(NIC) in water,sediment,fish muscle and skin in natural proportions and shrimp muscle.The water sample was extracted with ethyl acetate after alkalization treatment,and the other samples were extracted with acetonitrile containing 0.1% ammonia,and purified using C18 powder.The extracts were separated on a Thermo Hypersil Gold C18(150 mm×2.1 mm,5 μm) column with acetonitrile-water as mobile phase at a flow rate of 0.3 mL/min,then detected in selected reaction monitoring(SRM) mode and quantified by internal standard calibration curve method with the stable isotope marker of NIC(NIC-13C6) as internal standard.Results showed that good linearities for NIC in the samples were observed in the range of 0.2-200 μg/L,with their correlation coefficients(r2) not less than 0.999 5.The average recoveries for NIC in water at three spiked levels of 2.5,25 and 250 ng/L ranged from 90.5% to 109% with relative standard deviations(RSD) of 3.2%-11%.The limit of detection(LOD) and limit of quantitation(LOQ) for NIC in water were 1.0 ng/L and 2.5 ng/L,respectively.While for NIC in sediment,fish muscle and skin in natural proportions and Procambarus clarkii muscle,the average recoveries at three spiked levels of 0.5,5.0 and 50 μg/kg were in the ranges of 89.4%-113%,92.8%-110% and 94.1%-107%,with their RSDs of 4.6%-12%,2.8%-11% and 3.2%-9.3%,respectively.The LODs and LOQs were 0.2 μg/kg and 0.5 μg/kg,respectively.With high sensitivity,accuracy and selectivity,the present method is suitable for the determination of NIC residues in practical aquatic environmental water,sediment,fish and shrimp.

关 键 词：同位素稀释 氯硝柳胺 水体 底泥 鱼 虾 高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] F762.6[理学—化学]