通过型固相萃取-高效液相色谱-串联质谱法同时测定水产品中的5种硝基咪唑和地西泮  

Simultaneous Determination of Five Nitroimidazoles and Diazepam in Aquatic Products by High-Performance Liquid Chromatography- Tandem Mass Spectrometry With Pass-Through Solid Phase Extraction Purification

作　　者：何连军[1] 王鼎南 张宜明[2] 汪思佳 HE Lianjun;WANG Dingnan;ZHANG Yiming;WANG Sijia(Hangzhou Vocational and Technical College,Hangzhou,Zhejiang 310018;College of Agricultural and Food Sciences,Zhejiang A&F University,Hangzhou,Zhejiang 311300;Zhejiang Aquatic Technology Promotion Station,Hangzhou,Zhejiang 310023)

机构地区：[1]杭州职业技术学院,浙江杭州310018 [2]浙江农林大学,农业与食品科学学院,浙江杭州311300 [3]浙江省水产技术推广总站,浙江杭州310023

出　　处：《核农学报》2021年第8期1865-1874,共10页Journal of Nuclear Agricultural Sciences

基　　金：杭州市农业与社会发展计划项目(20191203B26);浙江省公益技术研究计划/分析测试项目(LGC20B050007)。

摘　　要：为建立一种同时检测水产品中5种硝基咪唑(甲硝唑、地美硝唑、洛硝哒唑、羟基甲硝唑、羟甲基甲硝咪唑)和地西泮的分析方法,本研究以通过型固相萃取柱Captiva EMR-Lipid(EMR)为净化手段,采用液相色谱-串联质谱法(HPLC-MS/MS)分析水产品中6种目标化合物的残留量。结果表明,样品经缓冲盐调节pH值,乙酸乙酯提取,EMR小柱净化,能有效去除基质干扰。6种目标化合物在在2-100 ng·mL^(-1)浓度范围内线性良好,相关系数r均不低于0.998,该方法在不同水产品基质中的加标回收率范围为87.7%-110.0%,相对标准偏差为0.63%-11.17%。经验证,本方法适用于多种水产品中5种硝基咪唑和地西泮的同时测定,方法简单可靠,可操作性强,适合于实验室内的大批量检测。In order to establish an analytical method for the simultaneous detection of 5 nitroimidazoles(metronidazole, dimenidazole, lonidazole, hydroxy metronidazole, hydroxymethyl metronidazole) and diazepam in aquatic products, a kind of pass-through solid-phase extraction column Captiva EMR-Lipid(EMR) was used to purify the six compounds in aquatic products, and the residual amount was analyzed by high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). The calibration curves of target compounds had good linearity within corresponding concentration ranges and the coefficient ≥ 0.998. Moreover, the average spiked recoveries were between 87.7% and 110.0%, with the relative standard deviations of 0.63% to 11.17%. It has been verified that the established method is suitable for simultaneously determining 5 nitroimidazoles and diazepam in aquatic products with variety of matrix. The method is simple, reliable, easy-to-operability, and is suitable for high-through tests in the laboratory.

关 键 词：通过型固相萃取 硝基咪唑 地西泮 水产品 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]