首页|液质联用测定福鼎白茶中高氯酸盐含量及其污染情况研究

液质联用测定福鼎白茶中高氯酸盐含量及其污染情况研究

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建立了液质联用测定福鼎白茶中高氯酸盐含量的分析方法,并采用该方法测定了39个福鼎白茶中的高氯酸盐残留量.白茶样品用65%甲醇水溶液提取,HLB和GCB固相萃取小柱净化,Waters IC-Pak AnIon HR色谱柱分离,乙腈-乙酸铵溶液作为流动相梯度洗脱,UPLC-MS/MS分析,同位素内标法定量.方法的检出限为8 μg/kg,定量限为25 μg/kg,满足欧洲食品安全委员会对茶叶中高氯酸盐临时安全限量值0.75 mg/kg的要求.在未污染的白茶样品中添加20、200、750 μg/kg高氯酸盐进行加标回收试验,回收率为87.5%~101.6%,相对标准偏差为(RSD,n=6)2.7%~11.2%.采用该方法测定39个福鼎白茶,结果显示白茶样品中高氯酸盐的检出值均低于欧盟临时限量0.75 mg/kg,福鼎白茶中高氯酸盐污染风险可控.
Study on the determination of perchlorate content and pollution in Fuding white tea by LC-MS/MS
An analytical method for the determination of perchlorate in white tea by LC-MS/MS was established.White tea samples were extracted with 65%methanol solution,purified with GCB and HLB,separated by Waters IC-Pak Anlon HR column,eluted with acetonitrile-ammonium acetate solution as mobile phase gradient,analyzed by UPLC-MS/MS,and quantified by isotope internal standard method.The limits of detection and quantitation were 8 μg/kg and 25 μg/kg respec-tively,which met the requirements of the European Food Safety Commission for the provisional safety limit of perchlorate in tea of 0.75 mg/kg.The recoveries of 20,200 and 750 μg/kg perchlorate were 87.5%-101.6%,and the relative standard devi-ations were(RSD,n=6)2.7%-11.2%.The results showed that the detected value of perchlorate in 39 white tea samples were all lower than the EU provisional limit of 0.75 mg/kg,and the risk of perchlorate contamination in white tea was con-trollable.

PerchlorateWhite teaUPLC-MS/MS

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宁德市产品质量检验所,福建 宁德 352100

高氯酸盐 白茶 UPLC-MS/MS

2024

福建分析测试
福建省测试技术研究所

福建分析测试

影响因子:0.365
ISSN:1009-8143
年,卷(期):2024.33(3)