液相色谱串联质谱法检测海产养殖用水中乙酰甲喹及其代谢物残留  

Determination of mequindox and its metabolites in mariculture water by liquid chromatography-tandem mass spectrometry

作　　者：尤艳莉[1] 李福翔 孙甲霖 李彦伸[1] YOU Yan-li;LI Fu-xiang;SUN Jia-lin;LI Yan-shen(College of Life Science,Yantai University,Yantai,Shandong 264000,China)

机构地区：[1]烟台大学生命科学学院,山东烟台264000

出　　处：《南方农业学报》2023年第1期238-249,共12页Journal of Southern Agriculture

基　　金：山东省自然科学基金面上项目(ZR2022MC214)。

摘　　要：【目的】建立一种准确、快速检测海产养殖用水中乙酰甲喹(MEQ)及其代谢物残留的方法,为海产养殖环境中的实际检测提供参考依据。【方法】使用超声辅助—分散液液微萃取(UA-DLLME)对海水样品中的MEQ及其代谢物残留进行富集,使用液相色谱串联质谱(LC-MS/MS)测定兽药残留物浓度。通过单因素试验和响应面法优化影响回收率的各项微萃取条件以获得最大回收率,并以最优条件应用于实际样品的测定。【结果】单因素优化试验确定四氯乙烷和甲醇作为萃取剂和分散剂;响应面优化试验确定最优萃取参数:萃取剂用量80μL,分散剂用量175μL,超声时间5.2 min,3个因素及萃取剂用量与分散剂用量、萃取剂用量与超声时间对回收率有显著影响(P<0.05);实际样品检测中均未检出MEQ残留,阳性对照试验的平均加标回收率为53.0%~93.0%,相对标准偏差为2.8%~12.7%;MEQ及其代谢物共8种化合物在1.0~500.0μg/L范围内线性良好,相关系数R2≥0.99500,方法检测限为0.022~0.170μg/L,定量限为0.073~0.567μg/L。【结论】建立的UA-DLLME与LC-MS/MS联用方法具有操作简单、灵敏度高、环境友好等特点,可用于海产养殖水中兽药MEQ及其代谢物残留量的快速检测。【Objective】To establish an accurate and rapid method for the detection of mequindox(MEQ)and its metabolites in mariculture water,provide a reference for the actual detection in mariculture environment.【Method】Ultrasonic assisted dispersive liquid-liquid microextraction(UA-DLLME)was used to enrich MEQ and its metabolites in seawater samples.Liquid chromatography-tandem mass spectrometry(LC-MS/MS)was used to determine the concentration of veterinary drug residue.The single factor optimization and response surface optimization were used to optimize the microextraction conditions affecting the recovery rate to obtain the maximum recovery rate,and the optimal conditions were applied to the determination of actual samples.【Result】Tetrachloroethane and methanol were selected as extractant and disperser by single factor optimization test.The optimal extraction parameters were determined by response surface optimization test as extractant volume 80μL,disperser volume 175μL,ultrasound time 5.2 min.Three factors,extractant dosage and disperser dosage,extractant dosage and ultrasonic time had significant effects on the recovery rate(P<0.05).No residue of MEQ was detected in actual samples,and the average recoveries of positive control experiments were 53.0%-93.0%,the relative standard deviations were 2.8%-12.7%.The linearities of MEQ and its metabolites were good in the range of 1.0-500.0μg/L,and the correlation coefficient R2≥0.99500.The limit of detections were 0.022-0.170μg/L.The limit of quantitations were 0.073-0.567μg/L.【Conclusion】UA-DLLME combined with LC-MS/MS has the characteristics of simple operation,high sensitivity and environmental friendliness,which can be used for the rapid detection of veterinary drug residues of MEQ and its metabolites in mariculture water.

关 键 词：超声辅助—分散液液微萃取 液相色谱串联质谱 海水 乙酰甲喹 回收率 

分 类 号：S912[农业科学—水产科学]