同位素稀释-超高效液相色谱-串联质谱法测定茶叶中的高氯酸盐

Detection of perchlorate in tea by ultra high performance liquid chromatography with tandem mass spectrometry and isotope dilution method

目的建立茶叶中高氯酸盐的超高效液相色谱-串联质谱测定方法。方法茶叶中高氯酸盐用0.2%乙酸提取,经石墨炭黑柱净化,优选Synergi^(TM)MAX-RP柱(4.6 mm×250 mm,4μm)为分析柱,以超高效液相色谱-串联质谱法测定,内标法定量。结果高氯酸盐在0.25~50.0μg/L范围内线性良好,回归方程y=1.569x+0.0268,相关系数r^2=0.999 6。加标浓度为0.05~0.50 mg/kg时,回收率95.6%~120.0%,相对标准偏差(RSD)1.9%~17.5%。检出限为2.5μg/kg。结论本方法前处理简单、准确、灵敏度高,适用于茶叶中高氯酸盐的测定。

Objective To establish a method for the determination of perchlorate in tea by ultra high performance liquid chromatography and tandem mass spectrometry. Methods The perchlorate residue in tea was extracted with 0. 2% acetic acid,and the supernatant was cleaned up with Carb SPE,the detection was performed by ultra high performance liquid chromatography tandem mass spectrometry with internal standard method for quantitative. Results The calibration curve was linear in the concentration range of 0. 25-50 μg / L（ r-2= 0. 999 6）,the recovery was in the range of 95. 6%-120. 0%,the relative standard deviation（ RSD） was in the range of 1. 9%-17. 5%,and the limit of detection of perchlorate was 2. 5μg /kg. Conclusion The method is suitable for the determination of perchlorate in tea with more simplicity,accuracy and high sensitivity.