建立了一种分散固相萃取-超高效液相色谱-串联质谱快速测定不同茶类中2,4-表芸苔素内酯的方法。样品经乙腈均质提取,通过C18、强阴离子交换剂（SAX）和石墨化碳黑（GCB）混合吸附剂分散萃取前处理,以HSS T3色谱柱分离,采用ESI正离子扫描和可编程多反应监测模式（SMRM）检测,基质匹配溶液外标法定量。2,4-表芸苔素内酯在0.8~800βμg·L-1范围内线性良好（R2>0.999）。在不同茶类（绿茶、红茶、白茶、黑茶、乌龙茶）中标准样含量20、40和200βμg·kg-1添加水平下,目标化合物回收率均介于75.5%~93.6%之间,相对标准偏差RSD值在0.4%~7.0%之间（n=6）,方法定量限（LOQ,S/N=10）在0.55~1.46βμg·kg-1之间。该方法稳定、准确、灵敏,能够满足各茶类检测需求。
诸力
,
陈红平
,
柴云峰
,
马桂岑
,
郝振霞
,
王晨
,
刘新
,
鲁成银
. 分散固相萃取-超高效液相色谱-串联质谱法测定不同茶类中2,4-表芸苔素内酯残留[J]. 茶叶科学, 2018
, 38(6)
: 589
-594
.
DOI: 10.13305/j.cnki.jts.2018.06.005
An efficient method for analyzing 2,4-Epibrassinolide in different teas was developed based on ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). Homogenized samples were extracted with acetonitrile solution, cleaned up with three sorbents including C18, strong anion exchanger (SAX) and graphitized carbon black (GCB). The compound was separated on a HSS T3 column using electrospray Ionization (ESI) mode, detected by scheduled multiple reaction monitoring (SMRM) and quantified by matrix-matched external standard curves. The compound showed good linearity between the concentration of 0.8-800βμg·L-1, with high significant correlation (R2>0.999). The limit of quantitation (LOQ, S/N=10) ranged from 0.55 to 1.46βμg·kg-1. In addition, the spiked (20, 40, 200βμg·kg-1) recoveries of tea samples were 75.5%-93.6%, and RSDs were 0.4%-7.0%. The method was accurately and sensitively applied to commercial tea samples, which fulfilled all requirement for the determination of 2,4-Epibrassinolide in tea samples.
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