高效液相色谱-串联四级杆质谱法测定保健食品中氯化高铁血红素  

Determination of hemin in food supplements by HPLC-MS/MS

作　　者：王超 张潇予 祝波 杨钊 WANG Chao;ZHANG Xiaoyu;ZHU Bo;YANG Zhao(Qingdao Institute for Food and Drug Control,Qingdao 266071)

机构地区：[1]青岛市食品药品检验研究院,青岛266071

出　　处：《中国食品添加剂》2023年第11期197-201,共5页China Food Additives

摘　　要：本研究旨在建立保健食品中氯化高铁血红素定性、定量测定的高效液相色谱-串联四级杆质谱方法,为加强氯化高铁血红素类保健食品的功效成分监督检查、规范其生产提供技术支持。供试品以2mL二甲亚砜为第一步提取溶剂,以甲醇为稀释溶剂,经Agilent ZORBAX Eclipse plus C_(18)RRHD色谱柱(3.0 mm×50 mm,1.8μm)分离,以0.1%的甲酸溶液-乙腈为流动相,在0.3 mL/min的流速下梯度洗脱。质谱采用ESI源的正模式条件下多反应监测模式,以保留时间和离子比率定性,以定量离子对峰面积进行外标法定量。氯化高铁血红素在线性范围内相关性较好,相关系数为0.9991;平均回收率为90.2%~98.5%,RSD为0.2%~0.3%;检出限为18 ng/g;定量限为54 ng/g。该方法专属性较好、灵敏度较高、检验快速准确,适用于保健食品中氯化高铁血红素的监督检测及质量控制。To establish a Liquid Chromatography-Mass Spectrometry(HPLC-MS/MS)method for determination of hemin in food supplements,and provide scientific knowledge for the regulation of hemin in food supplements.Samples were firstly extracted with 2 mL DMSO,diluted with methanol,and separated on Agilent ZORBAX Eclipse plus C_(18)Rapid Resolution HD column(3.0 mm×50 mm,1.8μm),with 0.1%formic acid and acetonitrile as mobile phase by gradient elution of 0.3 mL/min.The detection mode was positive by AJS ESI.Samples were identified with retention time and ion ratio,quantified with area of quantitative ion by ESTD method.Hemin showed good linear relationship within the range of corresponding concentrations.The correlation coefficient was 0.9991.The recoveries were within range of 90.2%~98.5%with RSD of 0.2%~0.3%.The detection limit was 18 ng/g,and the limit of quantification was 54 ng/g.The established method was specific,sensitive,rapid and simple for screening and determination of hemin in health food.

关 键 词：氯化高铁血红素 液相色谱质谱法 保健食品 多反应监测 

分 类 号：TS207.3[轻工技术与工程—食品科学]