超高效液相色谱-高分辨质谱法同时测定茶叶中15种吡咯里西啶类生物碱  

Simultaneous determination of pyrrolizidine alkaloids (PAs) in tea by ultra-high performance liquid chromatography-high resolution mass spectrometry

作　　者：许秀丽[1] 许博舟 王菡[1] 齐春艳 王秀娟[1] XU Xiuli;XU Bozhou;WANG Han;QI Chunyan;WANG Xiujuan(Chinese Academy of Inspection and Quarantine,Beijing 100176,China;Guangdong Institute of Food Inspection,Guangdong Guangzhou 510435,China)

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]广东省食品检验所,广东广州510435

出　　处：《中国食品卫生杂志》2021年第6期783-790,共8页Chinese Journal of Food Hygiene

基　　金：国家重点研发计划(2018YFC1602702)。

摘　　要：目的建立超高效液相色谱-高分辨质谱法同时测定茶叶中15种吡咯里西啶类生物碱(PAs)的分析方法。方法以甲醇甲酸水溶液作为提取溶剂,经超声提取,采用阳离子交换(MCX)固相萃取柱净化,以4.0 mmol/L甲酸铵溶液(含0.1%甲酸)和甲醇为流动相梯度洗脱,HSS T3柱(50 mm×2.1 mm, 1.7μm)分离,在正离子模式下采用高分辨质谱全扫描-数据非依赖性采集模式(Full MS/DIA)。结果基于数据采集结果,将吡咯里西啶类生物碱分为3类,筛选出3类不同的特征结构碎片离子。15种吡咯里西啶类生物碱在0.5~200μg/L的范围内线性关系良好(R^(2)>0.99),检出限和定量限分别为0.35~4.69μg/kg和1.18~11.17μg/kg。采用该方法对20例市售茶叶样品进行分析,1例菊花茶样品检出千里光碱,其余均低于方法检测低限。结论本方法灵敏度高、重现性好,可满足茶叶中15种吡咯里西啶类生物碱的测定要求。Objective To establish an analysis method for simultaneous determination of 15 kinds of pyrrolizidine alkaloids(PAs) in tea by ultra-high performance liquid chromatography-high resolution mass spectrometry. Methods Formic acid aqueous solution and methanol were used as extraction solvent. After the ultrasonic extraction and MCX solid phase extraction purification, the analytes were separated with HSS T3 chromatographic column(50 mm×2.1 mm, 1.7 μm) using 4.0 mmol/L ammonium formate solution(0.1% formic acidinclusive) and methanol as mobile phase for gradient elution. Finally, the eluents were determined by full scan/data independent acquisition(Full MS/DIA) of high resolution mass spectrometry in positive mode. Results Depending on the comprehensive data, the characteristic structural fragment ions of 3 kinds of PAs were screened out. Good linearities in the range of 0.5-200 μg/L were observed for 15 kinds of PAs(R^(2)>0.99), the limits of detection(LODs) and the limits of quantification(LOQs) were 0.35-4.69 μg/kg and 1.18-11.17 μg/kg, respectively. In this study, 20 commercial tea samples were analyzed using this method, and Jacobine was detected in 1 camomile tea sample, all the other measured values were lower than the LODs in the method. Conclusion This method has high sensitivity and stability, can meet the simultaneous detection requirements of 15 kinds of PAs in tea.

关 键 词：茶叶 超高效液相色谱-高分辨质谱 特征结构碎片离子 吡咯里西啶类生物碱 高通量筛查 

分 类 号：R155[医药卫生—营养与食品卫生学]