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

中文关键词:  分散固相萃取  液相色谱-串联质谱法  淡水鱼  磺胺  喹诺酮

英文关键词:dispersive solid phase extraction  liquid chromatography-tandem mass spectrometry  freshwater fish  sulfonamide  quinolone

中文摘要:

      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, 1.7 μm)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0.1~1.0 μg/kg、0.5~5.0 μg/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。

英文摘要:

      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, 1.7 μm), 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?1.0 μg/kg and 0.5?5.0 μg/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.