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建立了超高效液相色谱-串联质谱同时测定茶叶中高氯酸盐和氯酸盐的分析方法。选用ProElut C_(18)固相萃取柱对茶叶提取液进行净化、亲水性的Click Xion色谱柱分离,流动相A为水(含5 mmol·L~(-1)甲酸铵),流动相B为V_(甲醇)︰V_水=9︰1(含5 mmol·L~(-1)甲酸铵),甲酸调节pH至3.2,梯度洗脱分离,UPLC-MS/MS多反应监测(MRM)模式检测。该方法适用于茶叶中高氯酸盐和氯酸盐检测,平均回收率在60.5%~85.8%,RSD在4.9%~7.7%,高氯酸盐检出限为3mg·kg~(-1),氯酸盐检出限为5mg·kg~(-1)。方法操作简单、快速、灵敏度高,可以满足茶叶中高氯酸盐和氯酸盐的检测要求。
A method for simultaneous determination of perchlorate and chlorate in tea by ultra performance liquid chromatography-tandem mass spectrometry was established. The tea extract was purified with ProElut C_ (18) solid phase extraction column and separated by Click Xion. The mobile phase A was water (containing 5 mmol·L -1 ammonium formate), and the mobile phase B (Methanol): V_water = 9︰1 (containing 5 mmol·L -1 ammonium formate). The pH value of formic acid was adjusted to 3.2 with gradient elution. The UPLC-MS / Pattern detection. The method is suitable for the determination of perchlorate and chlorate in tea with the average recovery of 60.5% -85.8%, RSD of 4.9% -7.7%, the detection limit of perchlorate of 3 mg · kg -1, The detection limit of chlorate is 5 mg · kg -1. The method is simple, rapid and sensitive, which can meet the detection requirements of perchlorate and chlorate in tea.