建立了离子色谱-串联质谱检测茶叶中高氯酸盐的分析方法.选用高容量、强亲水性的IonPac AS2 0阴离子 交换柱(2 mm)进行分离,以淋洗液自动发生器在线产生的70 mmol/L 氢氧化钾为淋洗液等浓度淋洗, TSQ Quantiva三重四极杆质谱仪作检测器,采用电喷雾电离源负离子( E S r )模式、多反应监测( MRM)模式进行分析, 内标法定量.结果表明,高氯酸盐在0. 02-10. 0 μg/L 范围内线性关系良好,相关系数( r )为 0. 999 1,定量限为2 μg/kg.运用该方法测定5种茶叶中的高氯酸盐,加标回收率为87.3%-112.2%.该方法具有操作简单、专属性 强、灵敏度高等优点,可满足茶叶中高氯酸盐的检测要求.
A rapid ion chromatography-tandem mass spectrometry (IC-MS/MS) method was developed for the determination of perchlorates in tea. The chromatographic analysis was per-formed on Dionex 5000+,using high capacity and hydroxide selective column IonPac AS20 (2 mm). Perchlorates were separated by isocratic elution with 70 mmol/L KOH eluent generated from on-line eluent generation cartridge. TSQ Quantiva^TM,as a detector,scanned samples and monitored multi ion pairs simultaneously for confirmation and quantification,in the mode of negative ESI and multiple reaction monitoring (MRM). The results displayed good linearity in the range of 0. 02-10. 0 μg/L,with correlation coefficient (r ) of 0. 999 1. The relative standard deviations (RSDs) were 2. 67% (n = 5). The limits of quantification of the method were 2 μg/kg. The average recoveries of perchlorates in the five kinds of tea ranged from 87. 3% to 112. 2%. The results showed that the method is fast,simple,selective,sensitive and suitable for the determ nat on of perchlorates n var ous complex matr x samples such as tea.