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

Simultaneous Determination of Perchlorate and Chlorate in Tea by Ultra-peryethylene Liquid Chromatography-tandem Mass Spectrometry

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 using ultra high performance liquid chromatography-tandem mass spectrometry was developed for the determination of perchlorate and chlorate in tea. Tea extracts were purified by ProElut C18, separated by Click Xion column. The mobile phases were 5 mmol·L^-1 ammonium formate/water （A） and methanol： 5 mmol· L^-1 ammonium formate/water =9︰1 （B）. The pH was adjusted to 3.2 by formic acid and the samples were then analyzed by UPLC-MS/MS with multiple reaction monitoring mode （MRM）. The method was applied to detect perchlorate and chlorate in tea. The average recovery and relative standard deviations were in the range of 60.5%-85.8% and 4.9%-7.7%, respectively. The detecting limits of perchlorate and chlorate were 3μg·kg^-1 and 5μg·kg^-1, respectively. The method is simple, quick and high sensitive, which is suitable for the determination of perchlorate and chlorate in tea.