改进的QuEChERS结合LC-MS/MS同时测定蜂蜜中60种兽药残留

Simultaneous determination of 60 multi-residues of veterinary drugs in honey by modified QuEChERS and liquid chromatography-tandem mass spectrometry

建立了同时测定蜂蜜中60种兽药残留的LC-MS/MS检测方法。蜂蜜样品采用Mcllvaine缓冲溶液(pH 4)稀释,5%乙酸乙腈提取,提取液经盐析,NH2吸附剂分散固相萃取净化,LC-MS/MS动态多反应监控模式测定。在3个添加水平下(n=6),60种兽药平均回收率在70%～120%范围内的占比分别为96.7%,98.3%和98.3%,RSD为0.6%～20%。在0.1～1000μg/kg范围内,81.7%的目标物的线性相关系数(r2)>0.995,检出限和定量限范围分别为0.01～17.99μg/kg和0.02～59.97μg/kg。对16个市售蜂蜜样品进行测定,其中5个样品中检出磺胺类、喹诺酮类、硝基咪唑类等兽药残留。该方法具有一次处理样品,可同时测定60种兽药残留的特点,适合于蜂蜜中多类兽药的高通量筛查检测。

A novel method has been established for simultaneous determination of 60 veterinary drugs in honey by modified QuEChERS and liquid chromatography-tandem mass spectrometry. The honey sample was diluted with Mcllvaine buffer solution （ pH 4. 0）, and extracted with 5% acetic acid-acetonitrile. After elimination ofwater by salting out effect, the extract was purified by NH2 sorbent and the final solution was analyzed by LC-MS/ MS under dynamic multi-reaction monitoring mode. At three spiked levels （ n = 6）, the percentage of drugs with recoveries ranging from 70% to 120% were 96.7%, 98.3% and 98.3%, respectively. The relative standard deviations were between 0. 6% and 20%. The correlation coefficients for 81.7% of the veterinaries were larger than 0. 995 in the linear range of 0. 1 - 1000 μg/kg. Meanwhile, the ranges of the limits of detection and quantification were 0. 01 ~ 17.99 μg/kg and 0. 02 ~ 59.97 μg/kg, respectively. This method has been applied to the determination of veterinary drugs in 16 honey samples from market, and sulphonamides, quinolones, nitroimidazoles and other drugs have been detected in five samples. This simple, rapid and accurate method is suitable for high-throughput detection of multi-class veterinary drugs in honey.