超高效液相色谱-单四极杆质谱联用法检测奶粉与酸奶中33种兽药残留

Determination of 33 kinds of veterinary drugs residues in milk powder and yogurt by ultra performance liquid chromatography-quadrupole mass spectrometry

目的建立超高效液相色谱-单四极杆质谱(ultra performance liquid chromatography-quadrupole mass spectrometer, UPLC-QDa)同时测定奶粉及酸奶中33种(咪唑类、β受体激动剂和大环内酯类)兽药残留的检测方法。方法样品经水溶解分散后以3%(V:V)甲酸乙腈超声提取,离心后上清液用PRIME HLB固相萃取柱净化后氮吹浓缩,采用0.1%甲酸水溶液(A)和乙腈(B)作为流动相进行梯度洗脱,以选择离子监测模式对各个目标化合物定量离子进行监测分析。结果33种兽药在各自浓度范围内线性关系良好,相关系数均大于0.991。33种兽药在2种基质中的加标回收率为59.4%~108.5%,相对标准偏差(relative standard deviation, RSD)为1.68%~13.70%(n=6),检出限(S/N=3, limits of detection, LOD)和定量限(S/N=10, limits of quantification, LOQ)分别为0.06~4.66μg/kg和0.19~23.68μg/kg。结论该方法快捷简单,灵敏度高,适用于奶粉及酸奶样品中多种兽药检测。

Objective To establish a method for determination of the residues of 33 kinds of veterinary drugs (benzimidazoles,β-adrenergic receptors and macrolides) in milk powder and yogurt by ultra performance liquid chromatography-quadrupole mass spectrometry (UPLC-QDa). Methods The samples were dissolved in water and then extracted by ultrasonic with acetonitrile containing 3% formic acid (V:V). After the purification with solid phase extraction, the sample solutions were separated on a reversed phase using a gradient elution program of 0.1% formic acid aqueous solution (A) and acetonitrile solution (B). The selected ion monitoring mode was used to monitor and analyze the quantitative ions of each target compound. Results The 33 kinds of veterinary drugs had good linear relationships in their concentration range, with correlation coefficient were higher than 0.991. The recoveries at 3 spiked levels in 2 type of 33 samples were 59.4%-108.5%, with the relative standard deviations of 1.68%-13.70%(n=6). The limits of detection(LOD, S/N=3)and the limits of quantification(LOQ, S/N=10) were 0.06-4.66 μg/kg and 0.19-23.68 μg/kg, respectively. Conclusion This method is rapid, simple, sensitive, which suitable for the determination of the 33 veterinary drugs in milk powder and yogurt.