分散固相萃取结合液相色谱-串联质谱法测定淡水鱼中9种磺胺类和3种喹诺酮类药物残留量  

Determination of 9 kinds of sulfonamides and 3 kinds of quinolones residues in freshwater fish by dispersive solid phase extraction coupled with liquid chromatography-tandem mass spectrometry

作　　者：周瑞铮 陈锦杭 张树权 周惠健 郑耀林 林秋凤[1] ZHOU Rui-Zheng;CHEN Jin-Hang;ZHANG Shu-Quan;ZHOU Hui-Jian;ZHENG Yao-Lin;LIN Qiu-Feng(Dongguan Institutes for Food and Drug Control,Dongguan 523808,China)

机构地区：[1]东莞市食品药品检验所,东莞523808

出　　处：《食品安全质量检测学报》2021年第17期6946-6952,共7页Journal of Food Safety and Quality

摘　　要：目的建立分散固相萃取结合液相色谱-串联质谱法检测淡水鱼中9种磺胺类和3种喹诺酮类药物的分析方法。方法淡水鱼肉样品用1%甲酸乙腈提取,提取液经盐析后取乙腈层,用分散固相萃取净化包净化,目标物用C18色谱柱(2.1 mm×50 mm,1.7μm)分离,采用0.1%甲酸水-乙腈作为流动相进行梯度洗脱,利用电喷雾离子源正离子多反应监测模式进行测定,内标法定量。结果9种磺胺和3种喹诺酮类药物在1~50 ng/mL浓度范围内线性关系良好,相关系数均大于0.999。检出限和定量限分别为0.1~1.0μg/kg、0.5~5.0μg/kg,在3个不同浓度添加水平下的平均回收率为84.4%~114.6%,相对标准偏差为1.0%~7.8%(n=6)。结论该方法操作简单、快速、灵敏度高,适用于淡水鱼中常见9种磺胺和3种喹诺酮类兽药残留测定。Objective To establish a method for determination of 9 kinds of sulfonamides and 3 kinds of quinolones residues in freshwater fish by dispersive solid phase extraction coupled with liquid chromato graphy-tandem mass spectrometry.Methods Freshwater fish samples were extracted with 1%formic acid acetonitrile,the extracted solution was salted out,and the acetonitrile layer was purified with disperse solid phase extraction purification package,the target substance was separated on a C18 column(2.1 mm×50 mm,1.7μm),and gradient elution was carried out using water and acetonitrile with 0.1%formic acid as mobile phase,the electrospray ion source positive ion multi-reaction monitoring mode was used for determination,and the internal standard method was used for quantification.Results The 9 kinds of sulfonamides and 3 kinds of quinolones had good linear relationships in the concentration range of 1-50 ng/mL,and the correlation coefficients were all greater than 0.999.The limits of detection and limits of quantification were 0.1-1.0μg/kg and 0.5-5.0μg/kg,respectively,the average recoveries were 84.4%-114.6%at 3 kinds of different supplemental levels.The relative standard deviations were 1.0%-7.8%(n=6).Conclusion This method is simple,rapid,sensitive and suitable for the determination of 9 kinds of sulfonamides and 3 kinds of quinolones residues in freshwater fish.

关 键 词：分散固相萃取 液相色谱-串联质谱法 淡水鱼 磺胺 喹诺酮 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]