液相色谱-串联质谱法同时测定大黄鱼中20种磺胺类药物残留

Simultaneous Determination of Twenty Sulfonamide Residues in Yellow Larger Crocker by Liquid Chromatography Tandem Mass Spectrometry

建立了一种液相色谱-电喷雾串联质谱同时测定大黄鱼中20种磺胺类药物残留的方法。均质样品先后用乙腈、二氯甲烷提取,合并提取液,取部分提取液经氮吹浓缩。残渣用1 mL流动相溶解,饱和正己烷脱脂净化。采用ZORBAX Eclipse XDB-C8色谱柱,以含0.2%乙酸的水溶液和甲醇(7∶3)为流动相,梯度洗脱,在电喷雾-多反应监测离子模式下,进行定量定性分析。方法的定量限为5μg/kg;以标准加入法计算回收率,在10-40μg/kg添加范围内,平均回收率为79.6%-109%;相对标准偏差为3.55%-16.5%。

The method of simultaneous determination of twenty commonly used sulfonamide residues in Yellow Larger Crocker by liquid chromatography-electrospray tandem mass spectrometry （LC/MS/MS） is described. Sulfonamide residues were extracted from homogenized tissue with acetonitrile and dichloromethane. A part of the extract was taken and then dried by nitrogen. The residues were dissolved into 1 mL mobile phase and defatted with n-hexane （saturated by acetonitrile）. The twenty analytes were separated on ZORBAX Eclipse XDB-Cs Column with mobile phases containing methanol and 0.2% acetic acid and finally determined by electrospray ionization tandem mass spectrometry （ESI-MS-MS）. A linear gradient eluting program of methanol from 30% to 80% （V/V） was employed at a flow rate of 0.2 mL/min in 35 minutes. Analytes confirmation were performed using multiple reaction monitoring （ MRM ） with one precursor ion and two product ions as identifiers. The quantitative limit of mehtod was 5 g/kg. Recoveries tested by standard addition method were in the range of 79.6% - 109% , RSDs were in the range of 3.6% - 16.5% at a spiking level from 10 μ/kg to 40 μg/kg（n =6）.