高效液相色谱-串联质谱同位素内标法测定猪肉中5种磺胺类药物残留量
Determination of Five Types of Sulfonamides Residues in Pork by HPLC-MS/MS with Isotopic Internal Standard
李律雯 1刘燕 1伍宏凯 1梁祺琦 1高志敏 1伍绍登1
作者信息
- 1. 广东省农产品质量安全中心(广东省绿色食品发展中心),广东广州 510230
- 折叠
摘要
该方法采用高效液相色谱-串联质谱测定猪肉中5种磺胺类药物的残留量.猪肉样品经过乙腈提取,低温冷冻、高速离心脱脂,反向C18色谱柱分离,采用多反应监测正离子模式测定,使用同位素内标法定量.在优化条件下的结果显示,在5-200 ng/mL的质量浓度范围内线性良好,相关系数r均大于0.999.在空白猪肉样品中添加5、50、100、200 μg/kg水平的药物回收试验中,平均回收率在60%-110%之间,RSD在1.03%-8.07%之间(n=6).结果表明,此方法中样品的前处理简单,定量结果准确,重现性好,适用于猪肉中磺胺类药物残留的定性定量检测.
Abstract
Simultaneous calculation of 5 sulfonamides residues in pork was tested by high performance liquid chromatography-tandem mass spectroscopic method.The pork samples were extracted with actonitrile,defatted with deep-frozen and high-speed centrifugation,and then were separated by reversed phase C18 column,determined by multiple reaction monitoring positive ion mode,and quantified by isotope internal standard method.The linearity was good in the range of 5-200 ng/mL,and the correlation coefficients r was greater than 0.99.After adding reagents 5,50,100 and 200 μg/kg to pork samples,the average recoveries were 60%-110%,relative standard deviation RSD(relative standard deviation)results had been shown between 1.03%-8.07%(n=6).The method is simple,accurate and reproducible,which was suitale for qualitative and quantitative calculation of sulfonamides residues in pork.
关键词
猪肉/磺胺类药物/同位素内标法/高效液相色谱-串联质谱Key words
Pork/Sulfonamides/Isotopic internal standard method/High-performance liquid chromatography with tandem mass spectrometric(HPLC-MS/MS)引用本文复制引用
出版年
2024
NETL
NSTL
万方数据