响应面优化QuEChERS结合UHPLC-MS/MS法测定乌鳢肌肉中四环素类抗生素  

Response Surface Optimization of the QuEChERS Combined with UHPLC-MS/MS Method for Determination of Tetracyclines in Muscle of Channa argus

作　　者：李丽春[1,2,3] 刘书贵 林嘉薇[1,2,3] 尹怡 郑光明 赵城[1,2,3] 马丽莎 单奇[1,2,3] 戴晓欣 魏琳婷[1,2,3] 周豪 LI Lichun;LIU Shugui;LIN Jiawei;YIN Yi;ZHENG Guangming;ZHAO Cheng;MA Lisha;SHAN Qi;DAI Xiaoxin;WEI Linting;ZHOU Hao(Pearl River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Guangzhou 510380,China;Key Laboratory of Prevention and Control for Aquatic Invasive Alien Species,Ministry of Agriculture and Rural Affairs,Guangzhou 510380,China;Key Laboratory of Aquatic Animal Immune Technology of Guangdong Province,Guangzhou 510380,China)

机构地区：[1]中国水产科学研究院珠江水产研究所,广东广州510380 [2]农业农村部外来入侵水生生物防控重点实验室,广东广州510380 [3]广东省水产动物免疫技术重点实验室,广东广州510380

出　　处：《食品工业科技》2023年第21期216-226,共11页Science and Technology of Food Industry

基　　金：广州市科技计划项目(202102020983);国家水产品质量安全风险评估项目(GJFP201700903);广东省现代农业产业技术创新团队专项资金(2020KJ150)。

摘　　要：为了评估乌鳢中四环素类药物的残留风险,建立了乌鳢肌肉中4种四环素类药物残留的快速、简单、廉价、高效、耐用和安全的前处理方法(Quick、Easy、Cheap、Effective、Rugged、Safe,QuEChER)。采用Box–Behnken design(BBD)响应面优化法,优化了提取和净化条件。样品经10 mL 1%甲酸酸化乙腈和2 mL 0.1 mol/L Na2EDTA-McIlvaine缓冲溶液提取,以150 mg PSA和200 mg C18进行净化,采用超高效液相色谱-串联质谱法(Ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测。结果表明,该方法在0.50~100 ng/mL浓度范围内线性良好(r≥0.999),检出限(Limit of Detection,LOD)和定量限(Limit of Quantitation,LOQ)分别为0.25~0.75μg/kg和0.84~2.00μg/kg。在乌鳢肌肉中四环素、土霉素、金霉素和多西环素的平均回收率在89.5%~1187%之间,相对标准偏差(RSD)在1.11%~8.88%之间。该方法简便、灵敏、准确,可用于乌鳢中四环素含量的快速测定。A quick,easy,cheap,effective,rugged and safe pre-treatment method(QuEChERS)was established to evaluate the risk of tetracycline residues in the muscle of Channa argus.The Box-Behnken design(BBD)response surface optimization method was used to optimize the extraction and purification conditions.The samples were extracted with 10 mL acetonitrile(containing 1%formic acid)and 2 mL 0.1 mol/L Na2EDTA-Mcllvaine buffer solution,and the extracts were purified by 150 mg primary secondary amine(PSA)and 200 mg C18,and detected with Ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The result showed that the calibration curve was linear in the range of 0.50~100 ng/mL,with high correlation coefficients(r≥0.999).The limits of detection(LOD)and quantification(LOQ)were 0.25~0.75μg/kg and 0.84~2.00μg/kg,respectively.The average recoveries of tetracycline,oxytetracycline,chlortetracycline and doxycycline at three different spiked levels in the muscle of Channa argus were 89.5%~118%,with relative standard deviations(RSDs)of 1.11%~8.88%.This method is simple,sensitive and accurate,and can be used for the rapid quantitative determination of tetracyclines in Channa argus.

关 键 词：QUECHERS 超高效液相色谱-串联质谱 乌鳢 四环素类 风险评估 

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]