超高效液相色谱-质谱检测羊奶中八大类74种禁限用药物方法研究

目的：为有效防范羊奶中药物残留风险，采用超高效液相色谱-质谱法建立羊奶中β-受体激动剂、磺胺、喹喏酮、大环内酯、苯并咪唑、镇静剂、抗病毒和截短侧耳素类共八大类74种禁限用药物残留检测方法。方法：样品经过0.5%甲酸乙腈溶液提取，Oasis PRiME HLB柱净化后，经Acquity UPLC BEH C₁₈柱（100 mm×2.1 mm，1.7 μm）分离，以甲醇和0.1%甲酸溶液为流动相进行梯度洗脱，正离子多通道MRM信号采集模式，8大类药74种禁限用药物在10.5 min内分离完好。结果：在1.0~40.0 μg·L^-1浓度范围内，各类药物线性良好，相关系数均在0.991以上；羊奶中各类药物定量下限均低于0.5 μg·kg^-1，通过0.5、5.0、10.0 μg·kg^-1 3个浓度的添加回收试验表明，回收率在61.9%~119.7%，批内RSD为1.1%~17.6%，批间RSD为2.1%~18.5%。结论：方法的准确度及精密度满足GB/T 27404-2008技术要求。该方法弥补了现有国标方法同时检测药物种类少的缺点，对更全面筛查和确证羊奶中禁限用药物残留，监管羊奶质量安全具有一定的参考价值。

Objective: To effectively prevent the risk of drug residues in goat milk,and develope a multiresidue method based on ultra performance liquid chromatography-tandem mass spectrometry for the determination of eight categories of seventy four kinds of forbidden and restricted drug residues(β-agonists,sulfonamides,quinolones,macrolides,benzimidazoles,sedatives,antiviral drugs).Methods: Analytes were extracted by acidified acetonitrile,and purified by Oasis PRiME HLB SPE column.Seventy four forbidden and restricted drugs were analyzed by Acquity UPLC BEH C₁₈ column(100 mm×2.1 mm,1.7 μm)using methanol and 0.1% formic acid as the mobile phases.The signals were acquired through the multi-channel MRM mode and positive ion mode.All analytes could be well-separated by a gradient program during 10.5 minutes.Results: The calibration curves of seventy four forbidden and restricted drugs were linear in a concentration range of 1.0-40.0 μg·L^-1(r>0.991),and the limits of quantitation were all less than 1.0 μg·kg^-1 in goat milk.The recoveries of 1.0,10.0,20.0 μg·kg^-1 fortified samples ranged from 61.9% to 119.7%,with the intra-assay coefficient of variation of 1.1%-17.6% and the inter-assay coefficient of variation of 2.1%-18.5%.Conclusion: Compared with the existing national standard,the proposed method has the advantage of detecting the quantity of forbidden and restricted drugs in goat milk.In order to monitor the quality of goat,the proposed method has a certain reference value for more comprehensive screening and confirmation of forbidden and restricted drugs in goat milk.