同位素稀释超高液相色谱-串联质谱法测定鸡蛋中生物素含量  

Determination of biotin in egg by isotope dilution ultra performance liquid chromatography-tandem mass spectrometry

作　　者：卢兰香 薛霞 魏莉莉 公丕学 丁一 武传香 王骏 祝建华 刘艳明 LU Lanxiang;XUE Xia;WEI Lili;GONG Pixue;DING Yi;WU Chuanxiang;WANG Jun;ZHU Jianhua;LIU Yanming(Shandong Institute for Food and Drug Control,Jinan 250101)

机构地区：[1]山东省食品药品检验研究院,济南250101

出　　处：《分析试验室》2020年第8期914-918,共5页Chinese Journal of Analysis Laboratory

基　　金：国家食品安全关键技术研发重点专项(2017YEC1601600);山东省自然科学基金(ZR2017MC069)资助。

摘　　要：建立了同位素稀释超高液相色谱-串联质谱法测定鸡蛋中生物素含量的分析方法。样品采用0.1 mol/L H2SO4121℃水解30 min提取后,QASIS PRiME HLB固相萃取柱净化,经C18色谱柱分离,三重四极杆电喷雾质谱检测,内标法定量。生物素在0.5~25 ng/mL范围内线性关系良好(R^2=0.998);高、中、低3个加标水平的回收率在95.8%~110.8%之间,相对标准偏差范围小于4.6%。方法检出限(S/N=3)为0.75μg/100 g,定量限(S/N=10)为2.5μg/100 g。方法可为鸡蛋中生物素的含量水平测定和研究提供技术支持。An isotope dilution ultra performance liquid chromatography-tandem mass spectrometry method had been developed for the determination of biotin in eggs by solid phase extraction Purification(SPE).Samples were extracted by 0.1 mol/L sulfuric acid hydrolysis under 121℃ for 30 minutes and purified by QASIS PRi ME HLB column.The separation was carried out on a C18 column by ultra performance liquid chromatography(UPLC).The target compound was detected by MS/MS system with eletrospray ionization(ESI)under a multiple reaction monitoring(MRM)mode which was quantified by an internal standard method.This method showed good linearity of biotin with the correlation coefficients of R^2=0.998 in the concentration range from 0.5 to 25 ng/m L.The average recoveries for the target compound were between 95.8%-110.8% with RSDs less than 4.6%.The limit of detection and quantification for biotin were 0.75μg/100 g and 2.5μg/100 g,respectively.The developed method can provide a strong technical support for the determination of biotin and research of the nutritional value in eggs.

关 键 词：生物素 超高液相色谱-串联质谱 固相萃取 内标法 鸡蛋 

分 类 号：TS207.3[轻工技术与工程—食品科学]