高效液相色谱-串联质谱法测定调味品中7种对羟基苯甲酸酯类防腐剂及其水平调查  

Determination of Seven p-Hydroxybenzoate in Condiments Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：魏一婷 吴媛 丁琳 占永超 柳菡 丁涛 徐敦明 WEI Yiting;WU Yuan;DING Lin;ZHAN Yongchao;LIU Han;DING Tao;XU Dunming(Xiamen Customs Technology Center,Xu Dunming Employee Innovation Studio,Xiamen 361013;Nanjing Customs,Nanjing 210001)

机构地区：[1]厦门海关技术中心徐敦明职工技术创新工作室,福建厦门361013 [2]南京海关,江苏南京210001

出　　处：《分析科学学报》2023年第5期612-617,共6页Journal of Analytical Science

基　　金：福建省科技计划项目(2020I0032)。

摘　　要：建立了高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定调味品中7种对羟基苯甲酸酯类防腐剂(对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸异丙酯、对羟基苯甲酸丙酯、对羟基苯甲酸异丁酯、对羟基苯甲酸丁酯、对羟基苯甲酸庚酯)的方法。目标物质经乙腈提取,C_(18)色谱柱分离,电喷雾离子源(ESI)电离,采用外标法定量。结果表明,7种目标物质在2.0~200.0 ng/mL浓度范围线性关系良好,相关系数大于0.9990。方法定量限为0.005~0.05 mg/kg,检出限为0.002~0.02 mg/kg,回收率为70.2%~107.6%,相对标准偏差(RSD,n=6)为1.2%~10.6%。本方法采用质谱法负离子模式同时检测7种对羟基苯甲酸酯,满足一针进样同时测定,前处理方法简便,回收率高,可应用于调味品中7种对羟基苯甲酸酯的日常检测。A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the simultaneous determination of seven p-hydroxybenzoate preservatives(methyl p-hydroxybenzoate,ethyl p-hydroxybenzoate,isopropyl p-hydroxybenzoate,propyl p-hydroxybenzoate,isobutyl p-hydroxybenzoate,butyl p-hydroxybenzoate and heptyl p-hydroxybenzoate)in condiments.The samples were extracted with acetonitrile solution by dilution method,separated by C18 column,detected by negative ion MRM under ESI source,identified by retention time and characteristic ion pair,and quantified by external standard method.The results show that the linear relationship of the seven substances to be tested is good in the range of 2.0-200.0 ng/mL,and the correlation coefficient of quantitative ion pair is greater than 0.9990.The limits of detection(LODs,S/N≥3)were 0.002-0.02 mg/kg and the limits of quantification(LOQs,S/N≥10)were 0.005-0.05 mg/kg,and the recoveries were between 70.2%and 107.6%with the relative standard deviations of 1.2%-10.6%.This method uses mass spectrometry negative ion mode to detect 7 kinds of p-hydroxybenzoates at the same time,which meets the simultaneous determination of one needle injection.The method is simple and the recovery rate is high.It can be applied to the daily detection of 7 kinds of p-hydroxybenzoates in condiments.

关 键 词：调味品 对羟基苯甲酸酯防腐剂 高效液相色谱串联质谱法 

分 类 号：O657.63[理学—分析化学]