利用超高效液相色谱-高分辨四级杆飞行时间质谱联用技术,建立了一种快速筛查乳制品中8种氟喹诺酮5种磺胺类药物及其4种乙酰化代谢物的新方法。采用乙腈-20%三氯乙酸溶液(100：1, V/V, pH 2.0)作溶剂和Oasis HLB固相萃取载体作吸附剂,实现了牛奶样品中17种目标物的同时提取和有效净化。利用MassLynx Chromlynx软件建立了这17种分析物的数据库。以Full Scan/MSE进行定性筛查和定量检测。4种代谢物在10~2000μg/L范围内和其它分析物在0.5~100μg/L范围内,其基质匹配内标校准曲线呈现良好的线性(R2>0.983)。氟喹诺酮的定量限为0.5~0.8μg/kg,磺胺类药物及代谢物的定量限为0.5~13.0μg/kg。在3个添加水平分析物的平均回收率(69%~92%)在职业分析化学家协会( AOAC)提出的允许范围之内,相对标准偏差均小于15%。本方法快速而灵敏,成功用于乳制品中抗生素及其代谢物的筛查、确认和定量分析。所研究的每种药物及代谢物残留均低于有关的最高残留限量( MRLs),但某些乳制品中其总残留量已超过最高残留限量。%A novel analytical method employing ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry ( UPLC-Q-TOF/MS) was developed for the rapid screening of eight fluoroquinolones ( FQs) , five sulfonamides ( SAs) and four acetyled metabolites in dairy products. The simultaneous extraction and effective cleanup for seventeen target analytes in dairy product samples were achieved with acetonitrile-20% trichloroacetic acid (100:1, V/V, pH 2) as solvent and Oasis HLB SPE cartridges as sorbent. Using MassLynx Chromalynx Software, a database for 17 target analytes was established. Qualitatively screening and quantitative analysis were carried out by full scan/ MSE mode. The matrix-matched internal standard chalibration curves showed a good linearity (R2>0. 983) in the ranges of 10-2000 μg/L for metabolites and 0. 5-100 μg/L for other all antibioties. The limits of quantification were in the range of 0. 5-0. 8 μg/kg for FQs and 0. 5-13. 0 μg/kg for SAs and related metabolites. The average recoveries at three spiked levels were in the range of 69%-92%, which is within the acceptable range proposed by Association of Official Analytical Chemists ( AOAC) . The relative standard deviation was less than 15%. This novel approach had high speed and sensitivity, and was successfully applied to the screening, confirmation and quantification analysis of dairy products. The content of each analyte residue was much lower than the maximum residue limits ( MRLs) , but total content of multiresidue in some dairy product samples were more than the MRLs.
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