摘要
利用液相色谱-电喷雾串联质谱建立猪肉中13种磺胺类药物残留的同时、快速分析方法。猪肉样品中的残留药物用1%乙酸-乙腈均质提取,浓缩后用0.1%甲酸-乙腈定容,并用正己烷液-液分配除脂后,用Kinetex C18色谱柱(100mm×2.1mm,2.6μm)分离,以0.1%甲酸-乙腈作为流动相梯度洗脱,采用电喷雾正离子电离,多反应监测模式检测,基质匹配外标法定量。13种磺胺类药物在1～300μg/kg范围内线性关系良好,定量限均小于10μg/kg。在1、2μg/kg和10μg/kg这3个添加水平下,回收率在60.0%～78.1%之间,相对标准偏差(RSD)在0.24%～8.88%之间。此方法操作简便,灵敏度、准确度、精密度均满足残留分析的要求。
An HPLC-MS/MS method was developed for the simultaneous and rapid determination of thirteen sulfonamides in pork. Sulfonamide residues in samples were extracted with acidic acetonitrile. The extract was concentrated, defatted with hexane, filtered through a 0.22 }am filter membrane and transferred to a sample vial prior to HPLC-MS/MS analysis, Chromatographic separation was performed on a Kinetex C18 （100 mm X 2.1 mm, 2.6 μm） column using a gradient elution with water （0.1% formic acid） and acetonitrile as mobile phases. The mass spectrometer was operated using multiple reaction monitoring in positive ionization mode. All thirteen sulfonamides showed good linearity in the concentration range of 1 to 300 μg/kg, and the limit of quantification for each of the sulfonamides was below 10 μg/kg. The average recoveries from samples spiked at levels of 1, 2 and 10 μg/kg ranged from 60.1% to 78.1% with relative standard deviations of 0.24%--8.88%. The HPLC-MS/MS method is simple, sensitive, selective, and applicable for the routine simultaneous determination of sulfonamides in meat.
出处
《肉类研究》
2013年第2期13-17,共5页
Meat Research
基金
国家“973”计划项目(2012CB723705)
关键词
猪肉
磺胺
液相色谱
质谱
meat
sulfonamides
liquid chromatography
mass spectrometry
