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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 determination of perchlorate in tea by ultra performance liquid chromatography-tandem mass spectrometry. Methods The perchlorate in tea was extracted with 0.2% acetic acid and purified by graphite carbon black column (Synergi TM MAX-RP column 4.6 mm × 250 mm, 4 μm) Mass spectrometry, internal standard method. Results The perchlorate showed a good linearity in the range of 0.25-50.0 μg / L. The regression equation was y = 1.569x + 0.0268 with a correlation coefficient of r = 2 = 0.999 6. The recoveries ranged from 95.6% to 120.0% and the relative standard deviations (RSDs) ranged from 1.9% to 17.5% at spiking concentrations of 0.05-0.50 mg / kg. The detection limit was 2.5μg / kg. Conclusion The method pretreatment is simple, accurate, sensitive and suitable for the determination of perchlorate in tea.