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采用QuEChERS前处理方法和在线凝胶渗透色谱-气相色谱-质谱联用法(gel permeation chromatography-gas chromatography-mass spectrometry,GPC-GC/MS)快速测定鱼肉中9种羟基类兽药残留。采用在线凝胶色谱进行在线净化,除去鱼肉中大部分油脂,有效缩短了样品前处理时间,结合选择离子监测采集方式,可减少基质干扰,提高方法的选择性。样品经乙腈提取,分散基质固相萃取方式净化后,使用选择离子监测(SIM)模式检测,外标法定量。经方法学验证,9种羟基类兽药在0.5~20.0μg/L浓度范围内的线性关系良好,相关系数r大于0.99;样品的平均回收率为63.5%~90.2%,相对标准偏差为3.6%~15.4%,方法检出限为0.3~1.0μg/kg。将该方法应用于10批实际样品的检测,其中1批样品的氯霉素检测结果呈阳性,含量为6.1μg/kg。该方法灵敏度高、准确可靠,可用于鱼肉中9种羟基类兽药的定性定量分析。
Nine kinds of veterinary drug residues in fish meat were rapidly determined by QuEChERS pretreatment method and on-line gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC / MS). Online on-line gel chromatography purification, remove most of the fish oil, effectively reducing the sample pre-treatment time, combined with selective ion monitoring acquisition can reduce matrix interference and improve the selectivity of the method. The samples were extracted with acetonitrile and dispersed matrix SPE, and then detected by SIM mode and quantified by external standard method. The validation of the method showed that the linearity of 9 kinds of veterinary drugs in the concentration range of 0.5-20.0μg / L was good, the correlation coefficient r was greater than 0.99, the average recovery was 63.5% -90.2% and the relative standard deviation was 3.6% 15.4%, the detection limit was 0.3 ~ 1.0μg / kg. The method was applied to the detection of 10 batches of actual samples, of which 1 batch of samples showed a positive chloramphenicol test and the content was 6.1 μg / kg. The method has high sensitivity, accurate and reliable, and can be used for qualitative and quantitative analysis of nine kinds of veterinary drugs in fish.