QuEChERS-气相色谱质谱法快速测定水产饲料中地西泮残留  

Fast determination of Diazepam in Aquatic Feed by Gas Chromatography-Mass Spectrometry Combined with QuEChERS

作　　者：马丽莎[1] 尹怡[1] 谢文平[1] 单奇[1] 郑光明[1] 李丽春[1] 刘书贵[1] 戴晓欣[1] 赵城[1] 魏琳婷 林嘉薇 MA Lisha;YIN Yi;XIE Wenping;SHAN Qi;ZHENG Guangming;LI Lichun;LIU Shugui;DAI Xiaoxin;ZHAO Cheng;WEI Linting;LIN Jiawei(Pearl River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Key Laboratory of Prevention and Control for Aquatic Invasive Alien Species, Ministry of Agriculture and Rural Affairs/ Laboratory of Quality and Safety Risk Assessment for Aquatic Product (Guangzhou), Ministry of Agriculture and Rural Affairs,Guangzhou 510380, China)

机构地区：[1]中国水产科学研究院珠江水产研究所/农业农村部外来入侵水生生物防控重点实验室/农业农村部水产品质量安全风险评估实验室(广州),广东广州510380

出　　处：《中国渔业质量与标准》2022年第3期17-23,共7页Chinese Fishery Quality and Standards

基　　金：广东省渔业生态环境重点实验室开放基金项目(FEEL-2020-8);中国——东盟海上合作基金项目(CAMC—2018F)。

摘　　要：本研究以QuEChERS作为样品前处理手段,建立了测定水产品饲料中地西泮残留的气相色谱-质谱法(GC-MS)。样品经纯水和乙腈提取后加入无水硫酸钠除水及氯化钠盐析,提取液经吸附剂中性氧化铝、PSA、纳米二氧化锆结合GCB粉净化后上机检测,内标法定量。结果显示:地西泮在5~500μg/L质量浓度范围内线性关系良好,相关系数为0.9992,对配合饲料、浓缩饲料及饲料添加剂开展3个水平加标回收实验(0.15、0.25、0.50 mg/kg),方法加标回收率为86.3%~104.5%,相对标准偏差为1.4%~7.8%,地西泮的检出限为0.05 mg/kg,定量限为0.20 mg/kg,方法检出限远低于标准“NY/T 934—2005”的方法检出限1.00 mg/kg。该法具有前处理过程简单、快速、灵敏度高的优点,适合各种水产饲料中地西泮残留的测定。In this study,a gas chromatography-mass spectrometry(GC-MS)method was developed for the determination of diazepam in aquatic feed coupled with a quick,easy,cheap,effective,rugged and safe(QuEChERS)extraction technique for sample pretreatment.Anhydrous sodium sulfate was used for dehydration and sodium chloride was used for salting out after the extraction of samples by pure water and acetonitrile.Then the extracting solution was purified by neutral alumina,PSA,zirconium dioxide and GCB,followed by determination with internal standard method for quantification.The results showed that good linearity was obtained in the diazepam concentration range of 5-500μg/L,and the correlation coefficient was 0.9992.The recoveries of diazepam in the compound feed,concentrated feed and feed additives at three spiked levels of 0.15,0.25 and 0.50 mg/kg ranged from 86.3%to 104.5%with relative standard deviations(RSDs)of 1.4%-7.8%.The limit of detection(LOD)was 0.05 mg/kg and the limit of quantification(LOQ)was 0.20 mg/kg,that the LOD of the method was much lower than the LOD of 1.00 mg/kg established by“NY/T 934-2005”standard method.The method was suitable for the determination of diazepam in various aquatic feed with advantages of simple pretreatment process,rapid detection and high sensitivity.

关 键 词：气相色谱质谱法 稳定同位素内标 水产饲料 地西泮 QUECHERS 

分 类 号：O652.1[理学—分析化学]