超高效液相色谱法检测猪肉及其制品中的磺胺类及氟喹诺酮类兽药残留

Detection of sulfonamides and fluoroquinolones in pork and its products using ultra performance liquid chromatography

建立一种超高效液相色谱法(ultra-performance liquid chromatography,UPLC)同时检测猪肉中9种磺胺和3种氟喹诺酮类兽药残留的方法。以磷酸盐缓冲液(p H 6.0)为提取溶剂,提取猪肉糜中的磺胺类和氟喹诺酮类药物,提取液经HLB固相萃取柱净化和氮气浓缩吹干后,体积分数为20%甲醇水溶液定容至1 m L,以体积分数为0.1%甲酸水溶液和乙腈作为流动相,采用UPLC紫外串联荧光检测器检测。磺胺类和氟喹诺酮类药物分别在0.01~1.00μg/m L和0.001~0.200μg/m L范围内线性良好,相关系数均大于0.999,磺胺类检出限为1.2~3.5μg/kg,定量限为4.0~11.7μg/kg,氟喹诺酮类检出限为0.12~0.50μg/kg,定量限为0.4~1.7μg/kg,样品加标回收率为70.0%~98.0%,相对标准偏差(relative standard deviation,RSD)小于5%(n=6)。建立的UPLC方法可同时检测12种目标物,其峰形良好,检出限低,重现性好,准确度高,分析时间短,节省溶剂,能够满足肉及其制品中磺胺类及氟喹诺酮类药物的同时检测。

An ultra-performance liquid chromatography（ UPLC） method was developed for simultaneous detection of 9 kinds of sulfonamides and 3 kinds of fluoroquinolones in pork. Ground pork was extracted in phosphate solution（ p H = 6）,purified by HLB solid phase extraction column; after nitrogen drying at 40 ℃,20% methanol-water solution was used to dissolve to 1 m L; 0. 1% formic acid aqueous solution and acetonitrile were used as the mobile phasesolution,UV tandem fluorescence detectors was used as a detector. Sulfonamides and fluoroquinolones showed good linear in the range of 0. 01-1. 00 μg/m L,and 0. 001-0. 200 μg/m L,respectively,with the correlation coefficients above 0. 999. The limits of detection（ LOD） of sulfonamides were 1. 2-3. 5 μg/kg and the limits of quantitation（ LOQ） of sulfonamides were 4. 0-11. 7 μg/kg,the limits of detection（ LOD） of fluoroquinolones were 0. 12-0. 50μg/kg and the limits of quantitation（ LOQ） of fluoroquinolones were 0. 4-1. 7 μg/kg,the recoveries of spiked samples were between 70. 0%-98. 0% and the relative standard deviations（ RSD） was less than 5%（ n = 6）. The UPLC method established in this experiment can detect 12 kinds of targets simultaneously. This method exhibited good symmetrical peak shape,low detection limit,good reproducibility,high accuracy,short analysis time and fewer solvents. The method can be widely used for simultaneous detection of sulfonamides and fluoroquinolones in meat and its products.