PRIME HLB固相萃取-超高效液相色谱-串联质谱法测定水产品中5种硝基咪唑  

Determination of five nitroimidazoles residues in aquatic products by ultra-high performance liquid chromatography-tandem mass spectrometry coupled with PRIME HLB solid phase extraction

作　　者：马丽莎[1] 尹怡[1] 田斐 谢文平[1] 单奇[1] 刘书贵[1] 李丽春[1] 赵成 魏琳婷 戴晓欣[1] 郑光明[1] MA Lisha;YIN Yi;TIAN Fei;XIE Wenping;SHAN Qi;LIU Shugui;LI Lichun;ZHAO Cheng;WEI Linting;DAI Xiaoxin;ZHENG Guangming(Ministry of Agriculture and Rural Affairs Laboralon of Quality/Safety Risk Assessment for Aquatic Product(Guangzhou),Peail River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Guiingzhou 510380;Guiingdong Provincial Key Laljomtory of Fishery Ecology and Environment/South China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Guangzhou 510300)

机构地区：[1]中国水产科学研究院珠江水产研究所,农业农村部水产品质量安全风险评估实验室(广州),广州510380 [2]中国水产科学研究院南海水产研究所,广东省渔业生态环境重点实验室,广州510300

出　　处：《分析试验室》2021年第11期1304-1308,共5页Chinese Journal of Analysis Laboratory

基　　金：广东省渔业生态环境重点实验室开放基金(FEEL-2020-8);海南省热带海洋生物技术重点实验室开放基金(LTMB201904);中国-东盟海上合作基金(CAMC-2018F)项目资助。

摘　　要：建立了水产品中5种硝基咪唑类药物(洛硝唑、甲硝唑、异丙硝唑、地美硝唑、氯甲硝咪唑)残留量的超高效液相色谱-串联质谱测定方法。样品经乙酸铵缓冲液分散后,用0.1%氨水乙腈超声提取,提取液经PRiME HLB小柱及PSA吸附剂净化后,UPLC-MS/MS检测,基质匹配标准曲线内标法定量。结果表明,水产品中5种硝基咪唑类药物的平均回收率在83.5%~110.3%之间,相对标准偏差在1.9%~12%之间,在0.5~10 ng/mL线性范围内,线性相关系数(r^(2))均大于0.997,检出限为0.5μg/kg,定量限为1.5μg/kg。该方法能满足水产品中硝基咪唑类残留的检测需求。An ultra-high performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS) method for the detection of residues of 5 nitroimidazoles( ronidazole,metronidazole,ipronidazole,dimetridazole and chloromethylnidazole) in aquatic products was established. The samples were ultrasonically extracted with 0. 1%ammonia-acetonitrile solution,dispersed in ammonium acetate buffer,purified by PRi ME HLB column and PSA adsorbent,and determined by UPLC-MS/MS method. The analyte was quantified with internal standard using the matrix-matched standard calibration method. The results showed that the average spiked recoveries of 5 kinds of nitroimidazoles in aquatic products were 83. 5%-110. 3% with the relative standard deviations( RSDs) of 1. 9%-12%. Good linearities were obtained in the range of 0. 5-10 ng/m L,and the correlation coefficients were greater than 0. 997,the LODs were 0. 5 μg/kg,and the LOQs were 1. 5 μg/kg. The method could be used for the routine analysis of nitroimidazole residues in aquatic products.

关 键 词：水产品 硝基咪唑类 残留 PRiME HLB小柱 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]