摘要
目的采用超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定功能性饮料中的多种非法添加化学药物,为监管部门对食药品安全突发事件的快速应急处理提供技术保障。方法收集福建省2023年市售功能性饮料样品183批次,通过优化质谱参数、流动相,优化提取净化方法、净化材料、全自动QuEChERS试验方案,考察基质效应(matrix effect,ME),采用UPLC-MS/MS进行检测。采用t检验比较不同添加浓度下的检测方法,以评估回收率和相对标准偏差。结果40种非法添加化学药物在相应浓度范围内线性良好,相关系数r为0.9928~0.9999,最低检出限为0.001~0.048mg/kg,在定量限、2倍定量限和10倍定量限添加浓度下,方法平均回收率为61.6%~104.7%,相对标准偏差为0.8%~14.8%。183份样品中8批次样品检出番泻苷A或番泻苷B,检出率为4.4%。阳性样品中番泻苷A和番泻苷B的最高检出含量分别为60.8mg/kg和73.1mg/kg。在定量限、2倍定量限和10倍定量限添加浓度下,检测方法的回收率(t=14.25、16.70、17.03,均P<0.01)和相对标准偏差(t=10.19、12.97、13.06,均P<0.01)差异均有统计学意义。结论UPLC-MS/MS检测方法操作简便、灵敏度高、选择性好、定量准确、检测周期短,可应用于功能性饮料中多种非法添加化学药物的快速检测和确证。
Objective To simultaneously detect a variety of illegally added chemical drugs in functional beverages by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),and to provide a technical guarantee for the rapid emergency response of the supervisory department to food and drug safety emergencies.Methods A total of 183 batches of market sale functional beverage samples sold in Fujian Province in 2023 were collected.By optimizing the mass spectrometric parameters,mobile phase,optimize extraction and purification methods,purification materials,and fully automatic QuEChERS test protocol,investigate the matrix effect(ME),and detected using UPLC-MS/MS.The recovery and relative standard deviation were assessed by comparing detection methods at different addition concentrations using the t-test.Results The 40 illegally added chemical drugs showed good linearity in the corresponding concentration range with the coefficient r ranged from 0.9928 to 0.9999,and the lowest detection limit was from 0.001 to 0.048mg/kg.The recovery rate of the detection method was 61.6%-104.7%,and the relative standard deviation RSD was 0.8%-14.8%,under the limit of quantitation,2 times of limit of quantitation,and 10 times of limit of quantitation added concentrations.Sennoside A or sennoside B was detected in 8 batches out of 183 samples,with a detection rate of 4.4%.The highest detected contents of sennoside A and sennoside B in the positive samples were 60.8mg/kg and 73.1mg/kg,respectively.At the limit of quantitation,2 times of limit of quantitation,and 10 times of limit of quantitation addition concentrations,the differences in the recovery rates(t=14.25,16.70,17.03,all P<0.01)and relative standard deviations(t=10.19,12.97,13.06,all P<0.01)of the detection method were statistically significant.Conclusion UPLC-MS/MS detection method is easy to operate,with high sensitivity,good selectivity,accurate quantification and short detection cycle,which can be applied to the rapid detection and confirmation of a variety of ille
作者
石焱芳
王征
黄芊
王瑞娜
吴丽荣
黄颖芬
SHI Yanfang;WANG Zheng;HUANG Qian;WANG Ruina;WU Lirong;HUANG Yingfen(Quanzhou Medical College,Quanzhou,Fujian 362000,China;不详)
出处
《医学动物防制》
2024年第12期1167-1175,1181,共10页
Journal of Medical Pest Control
基金
福建省市场监督管理局科技项目(FJMS2020005)
泉州市科技局指导性科技计划项目(2021N132S)。
