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。
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.
出处
《食品工业科技》
CAS
CSCD
北大核心
2011年第11期426-430,共5页
Science and Technology of Food Industry
基金
山西省科技攻关计划(20110313024)
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
ultra high performance liquid chromatography tandem mass spectrometry
immunoaffinity
pork
egg
sulfonamides
