超高效液相色谱-四极杆飞行时间质谱法测定保健食品中的缓泻剂  

Determination of Laxatives in Health Food by Ultra Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry

作　　者：邓颖 林森煜 何敏恒 杜伟锋 张瑞瑞 区硕俊 DENG Ying;LIN Senyu;HE Minheng;DU Weifeng;ZHANG Ruirui;OU Shuojun(Guangzhou Inspection and Testing Certification Group Co.,Ltd.,National Quality Testing Center for Processed Food(Guangdong),Guangzhou 511447,China;Guangzhou Customs Technology Center,Guangzhou Key Laboratory of Import and Export Technical Measures of Animal,Plant and Food,Guangzhou 510623,China)

机构地区：[1]广州检验检测认证集团有限公司,国家加工食品质量检验中心(广东),广东广州511447 [2]广州海关技术中心,广东省动植物与食品进出口技术措施研究重点实验室,广东广州510623

出　　处：《现代食品》2021年第19期207-211,共5页Modern Food

摘　　要：目的:建立固相萃取柱净化,同时测定保健食品中的3种缓泻剂的超高效液相色谱-四极杆飞行时间质谱法。方法:样品经乙腈-水提取后,C_(18)固相萃取柱净化,氮气浓缩后乙腈复溶解。采用电喷雾电离源(ESI)进行电离,选择响应较好的碎片定性定量。结果:3种缓泻剂的标准曲线在2.0~200μg·L^(-1)的浓度内线性关系良好,相关系数r^(2)均在0.9989以上,加标回收率在84.6%~95.3%,相对标准偏差(RSD)为3.63%~6.22%,方法检出限(LOD)为7.0~20μg·kg^(-1),方法定量限(LOD)为20~50μg·kg^(-1)。结论:方法回收率好,重现性高,线性方程和检出限、定量限均可满足测定的要求。Objective:A simultaneous determination method for three laxatives in health food by solid phase extraction column purification coupled with ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry was established.Method:After the sample was extracted with acetonitrile-water,it was purified with a C_(18) solid phase extraction column,then concentrated by nitrogen and finally redissolved by acetonitrile.Electrospray ionization was used for ionization and fragments with better response were selected for qualitation and quantitation.Result:The standard curves of the three laxatives had a good linear relationship within the concentration of 2.0~200μg·L^(-1),while the correlation coefficient r^(2) were above 0.9989.The recovery rate of standard addition is 84.6%~95.3%,the relative standard deviation were ranged from 3.63%to 6.22%.The method limit of detection were 7.0~20.0μg·kg^(-1),and the method limit of quantitation were 20~50μg·kg^(-1).Conclusion:The method has good recovery rate and high reproducibility.The linear equation,limit of detection and limit of quantitation could satisfy the requirements of determination.

关 键 词：固相萃取柱 超高效液相色谱-四极杆飞行时间质谱 保健食品 缓泻剂 

分 类 号：O657.7[理学—分析化学]