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 C18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5βmmol·L-1甲酸铵）,流动相B为V甲醇︰V水=9︰1（含5βmmol·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3βμg·kg-1,氯酸盐检出限为5βμg·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。
Abstract
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 5βmmol·L-1 ammonium formate/water (A) and methanol: 5βmmol·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 3βμg·kg-1 and 5βμg·kg-1, respectively. The method is simple, quick and high sensitive, which is suitable for the determination of perchlorate and chlorate in tea.
关键词
茶叶 /
超高效液相色谱-串联质谱 /
高氯酸盐 /
氯酸盐
Key words
chlorate /
perchlorate /
tea /
ultra high performance liquid chromatography-tandem mass spectrometry
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基金
浙江省食品药品监管系统科技计划项目（SP201617）
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