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作 者:邵瑞婷 丁学妍 SHAO Ruiting;DING Xueyan(Beijing Institute of Food Inspection and Research(Beijing Municipal Center for Food Safety Monitoring and Risk Assessment),Laboratory of Key Technologies of Major Comprehensive Guarantee of Food Safety for State Market Regulation,Beijing 100041,China)
机构地区:[1]北京市食品检验研究院(北京市食品安全监控和风险评估中心),国家市场监管重点实验室食品安全重大综合保障关键技术,北京100041
出 处:《分析测试技术与仪器》2024年第2期76-85,共10页Analysis and Testing Technology and Instruments
摘 要:建立了一种检测保健茶中58种非法添加物的超高效液相色谱-串联质谱(UPLC-MS/MS)方法.样品经甲醇提取,超声离心后,取上清液经QuEChERS管(5982-4921)净化,UPLC-MS/MS测定,质谱采集模式为多反应监测电喷雾正离子模式(ESI+),基质外标法定量.在ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.8µm)反相柱上分离,梯度洗脱,流动相为乙腈和5 mmol/L乙酸铵+0.1%甲酸水溶液.在质量浓度为0.25~10 ng/mL范围内,各目标物标准品均呈现良好线性关系,相关系数平方(R^(2))均不小于0.985,检出限和定量限范围分别为0.005~0.050µg/g和0.01~0.10µg/g,回收率在60.2%~119.5%之间.方法对复杂的保健茶基质有良好的净化效果,具有前处理操作简单、重现性好、灵敏度高、杂质干扰小等特点,适用于保健茶中多种非法添加物的检测,可为保健品的质量安全监管提供技术支持.An ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the detection of 58 illegal additives in health tea was been established.The samples were extracted by methanol,and after ultrasonic centrifugation.The supernatant was purified by a QuEChERS(5982-4921)tube and determined by UPLC-MS/MS.The acquisition mode of mass spectrometer was multiple reaction monitoring electrospray ionization(ESI+),and quantified by matrix external standard method.Separation was performed on an ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.8μm)reversed-phase column with gradient elution,and the mobile phase was acetonitrile and 5 mmol/L ammonium acetate+0.1%formic acid solution.In the concentration range of 0.25~10 ng/mL,all the standard objects showed good linear relationships,and the correlation coefficient(R^(2))was greater than 0.985,the limits of detection and limits of quantitative were 0.005~0.050μg/g and 0.01~0.10μg/g,respectively,the recoveries ranged from 60.2%to 119.5%.The method has a good purification effect on the complex health tea matrix,and has the characteristics of simple operation,good reproducibility,high sensitivity and low interference of impurities.It is suitable for the detection of various illegal additives in health tea, and can provide a technical support for the quality and safety supervision of health products.
关 键 词:保健茶 QuEChERS净化 超高效液相色谱-串联质谱 非法添加
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