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

doi:10.13305/j.cnki.jts.2018.06.005

茶叶科学 ›› 2018, Vol. 38 ›› Issue (6): 589-594.doi: 10.13305/j.cnki.jts.2018.06.005

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

诸力, 陈红平, 柴云峰, 马桂岑, 郝振霞, 王晨, 刘新^*, 鲁成银^*

农业农村部茶叶质量监督检验测试中心,中国农业科学院茶叶研究所,农业农村部茶叶产品质量安全风险评估实验室（杭州）,农业部茶叶质量安全控制重点实验室,浙江杭州 310008

收稿日期:2018-04-28 修回日期:2018-08-03 出版日期:2018-12-15 发布日期:2019-12-15
通讯作者: *liuxin@tricaas.com;lchy@tricaas.com
作者简介:诸力,男,助理研究员,主要从事茶叶质量安全与风险评估研究。
基金资助:
国家现代农业产业技术体系（CARS-19）、国家自然科学基金（No. 31671941）、中国农业科学院创新团队茶叶质量与风险评估团队（CAAS-ASTIP-2014-TRICAAS-06）

Determination of 2,4-Epibrassinolide in Different Teas by Ultra Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry with Dispersive Solid Phase Extraction

ZHU Li, CHEN Hongping, CHAI Yunfeng, MA Guicen, HAO Zhenxia, WANG Chen, LIU Xin^*, LU Chengyin^*

Tea Quality and Supervision Testing Center, Ministry of Agriculture and Rural Affairs, Tea Research Institute, Chinese Academy of Agricultural Sciences, Laboratory of Quality and Safety Risk Assessment for Tea, Ministry of Agriculture and Rural Affairs (Hangzhou), Key Laboratory of Tea Quality and Safety Control, Ministry of Agriculture and Rural Affairs, Hangzhou 310008, China

Received:2018-04-28 Revised:2018-08-03 Online:2018-12-15 Published:2019-12-15

摘要/Abstract

摘要： 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。

关键词: 茶叶, 2, 4-表芸苔素内酯, 天丰素, 油菜素甾醇, 超高效液相色谱串联质谱, 分散固相萃取

Abstract: 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.

Key words: tea, 2, 4-Epibrassinolide, brassinolide, brassinosteroids, ultra performance liquid chromatography- tandem mass spectrometry, dispersive solid phase extraction

中图分类号:

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.

ZHU Li, CHEN Hongping, CHAI Yunfeng, MA Guicen, HAO Zhenxia, WANG Chen, LIU Xin, LU Chengyin. Determination of 2,4-Epibrassinolide in Different Teas by Ultra Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry with Dispersive Solid Phase Extraction[J]. Journal of Tea Science, 2018, 38(6): 589-594. doi: 10.13305/j.cnki.jts.2018.06.005.

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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

Determination of 2,4-Epibrassinolide in Different Teas by Ultra Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry with Dispersive Solid Phase Extraction

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