离子色谱-串联质谱法测定茶叶中的氯酸盐和高氯酸盐

Determination of chlorate and perchlorate in tea by ion chromatography-tandem mass spectrometry

利用离子色谱-串联质谱技术测定茶叶中氯酸盐、高氯酸盐的含量,通过优化提取条件和色谱-质谱等参数,在茶叶经纯水提取,固相萃取净化后,用离子色谱-质谱负离子模式进行定性、内标法定量分析。结果表明,氯酸盐在0.08~200 ng/mL、高氯酸盐在0.04~100 ng/mL范围内线性良好,相关系数均大于0.999,氯酸盐、高氯酸盐检出限分别1.0、0.5μg/kg,定量限分别为4.0、2.0μg/kg,加标回收率为80.0%~107.9%,相对标准偏差为0.47%~12.3%。所建方法检出限低,精密度良好,可准确定性和定量茶叶中氯酸盐和高氯酸盐的含量,为我国茶叶的风险监测提供了一种有力的技术手段。

The content of chlorate and perchlorate in tea is determined by ion chromatography-tandem mass spectrometry.After optimizing the extraction conditions and the parameters of chromatography-mass spectrometry,the tea samples are first extracted with pure water,followed by purification by solid-phase extraction.Finally,the negative ion mode of ion chromatography-mass spectrometry is used for qualitative analysis and quantitative analysis by internal standard method.The results show that the linearity of chlorate in the range of 0.08~200 ng/mL and perchlorate in the range of 0.04~100 ng/mL are good,and R 2 are higher than 0.999.The detection limits of chlorate and perchlorate are 1.0 and 0.5μg/kg,respectively.The quantitation limits for chlorate and perchlorate are 4.0 and 2.0μg/kg.The recoveries are in range of 80.0%~107.9%and RSDS ranges from 0.47%~12.3%.The method is simple,accurate,sensitive,which can accurately qualitatively and quantitatively determine the content of chlorate and perchlorate in tea,and provides a powerful technical means for the risk monitoring of tea in China.