分散固相萃取净化离子色谱-串联质谱测定茶叶中高氯酸盐

Determination of perchlorate in tea by dispersive solid phase extraction purification and ion chromatography-tandem mass spectrometry

中文关键词:  离子色谱-串联质谱法  高氯酸盐  茶叶

英文关键词:Ion chromatography-tandem mass spectrometry  perchlorate  tea

中文摘要:

      目的 建立分散固相萃取净化离子色谱-串联质谱法测定茶叶中高氯酸盐的含量。方法 样品经80 ℃超纯水浸泡提取30 min, 定性滤纸过滤, 滤液采用分散固相萃取技术, 以多壁碳纳米管和N-丙基乙二胺键合固相吸附剂吸附提取液中的杂质, 待测样品由离子色谱-串联质谱法测定, 内标法定量。结果 高氯酸盐浓度0.02~10.00 μg/L有良好的线性关系, 相关系数r2为0.9998, 检出限为0.6 μg/kg, 定量限为2.0 μg/kg, 加标回收率为80.1%~99.2%, 相对标准偏差为3.89%~7.68% (n=6)。对市场上随机购买的茶叶样品进行测定, 样品的含量为0.15~0.72 mg/kg。结论 该方法简便、可靠、稳定、灵敏度高, 可用于茶叶中高氯酸盐快速检测。

英文摘要:

      Objective To establish a method for the determination of perchlorate in tea by dispersive solid phase extraction purification and ion chromatography-tandem mass spectrometry. Methods The samples were extracted 30 min by ultra-pure water at 80 ℃ , filtered by qualitative filter paper, and purified by multi-walled carbon nanotubes and primary-secondary amine as dispersive solid-phase extraction sorbent. The samples were determined by ion chromatography-tandem mass spectrometry and were quantified by internal standard method. Results Perchlorate had good linear relationships in the range of 0.02?10.00 μg/L, and the correlation coefficients were 0.9998. The limit of detection was 0.6 μg/kg and the limit of quantitation was 2.0 μg/kg. The recoveries were 80.1%?99.2%, with the relative standard deviations of 3.89%?7.68%(n=6). The tea samples randomly purchased in the market were determined with the content of 0.15-0.72 mg/kg. Conclusion The method is simple, reliable, stable and sensitive, and can be used for rapid detection of perchlorate in tea.