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当前位置: 首页 > 文章 > 免疫亲和净化-超高效液相色谱串联质谱法同时测定猪肉和鸡蛋中的12种磺胺类药物 食品工业科技 2011 (11) 426-430
Position: Home > Articles > Immunoaffinity chromatography purification and ultra high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of twelve kinds of sulfonamides in pork and egg Science and Technology of Food Industry 2011 (11) 426-430

免疫亲和净化-超高效液相色谱串联质谱法同时测定猪肉和鸡蛋中的12种磺胺类药物

作  者：
赵笑天;潘亚利;傅英文;宋欢;林勤保
单  位：
山西大学应用化学研究所;山西出入境检验检疫局技术中心
关键词：
超高效液相色谱-串联质谱法;免疫亲和;猪肉;鸡蛋;磺胺类药物
摘  要：
建立了猪肉和鸡蛋中12种磺胺类药物的免疫亲和净化-超高效液相色谱串联质谱的确证方法。样品用超声提取后,直接过磺胺类药物免疫亲和净化柱净化;氮气吹干后用1∶9(v/v)的甲醇/水溶液定容,超高效液相色谱-串联质谱(UPLC-MS/MS)测定,电喷雾正离子(ESI+)、多反应模式下监测;实验结果表明,样品中磺胺类药物浓度在10～200μg/kg范围内时与其峰面积成良好线性关系,仪器检出限为0.4～2.0μg/L,方法的检出限为1.0～5.0μg/kg,3个加标水平下平均回收率为67%～100%,相对标准偏差为0.9%～10.0%,符合痕量分析的要求。
译  名：
Immunoaffinity chromatography purification and ultra high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of twelve kinds of sulfonamides in pork and egg
作  者：
ZHAO Xiao-tian1,PAN Ya-li2,FU Ying-wen2,SONG Huan2,LIN Qin-bao1,(1.Institute of Applied Chemistry,Shanxi University,Taiyuan 030006,China;2.Shanxi Entry-Exit Inspection and Quarantine Bureau,Taiyuan 030024,China)
关键词：
ultra high performance liquid chromatography tandem mass spectrometry;immunoaffinity;pork;egg;sulfonamides
摘  要：
A simultaneous determination method for twelve kinds of sulfonamides in pork and egg was developed using immunoaffinity chromatography(IAC)and ultra-high performance liquid chromatography-tendem mass spectrometry(UPLC-MS/MS).Samples were ultrasonicated extracted,and then the extracts were pooled and cleaned up with immunoaffinity column,followed by blowing to dryness under nitrogen gas stream,reconstitution with methanol/water mixture(1∶ 9,v/v)before the analysis on UPLC-MS/MS.The MS conditions used were positive(ESI+)electrospray ionization and MRM models.The results indicated as follows:All the studied sulfonamides had good linear relationship with peak area over the range from 10μg/kg to 200μg/kg,the detection limits of instrument for them ranged from 0.4μg/L to 2.0μg/L and the detection limits of method for them ranged from 1.0μg/kg to 5.0μg/kg;and the average recoveries rates in the above two matrices spike at three levels were between 67% and 100%,with relative standard deviations(RSDs)varying from 0.9% to 10.0%.This analytical method meets the requirements for trace assays.

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