基质分散固相萃取联合在线凝胶渗透色谱-气相色谱-串联质谱法测定湖南省市售茶叶中9,10-蒽醌的含量

doi:10.3969/j.issn.1006-3110.2022.10.008

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摘要目的建立基质分散固相萃取(quick,easy,cheap,effective,rugged and safe,QuEChERS)联合在线凝胶渗透色谱-气相色谱-串联质谱(gel permeation chromatography- gas chromatography-mass/mass spectrometry, GPC-GC-MS/MS)测定茶叶中9,10-蒽醌含量的快速检测方法,并对湖南省内市售茶叶进行9,10-蒽醌残留量检测和结果分析。方法茶叶中的9,10-蒽醌以1:1环己烷-乙酸乙酯提取后,经QuEChERS方法净化,进GPC-GC-MS/MS联用仪分析检测,以同位素d8-蒽醌内标法定量。结果茶叶中的9,10-蒽醌在1~100 μg/L浓度范围内与峰面积呈良好的线性关系,线性方程为y=0.0311x-0.0023,相关系数r=0.9997,方法的检出限为2 μg/kg,检测限为5 μg/kg;加标回收率为75.8%～98.4%,相对标准偏差2.6%～6.6%(n=6)。对湖南省14个地州市市售茶叶进行检测,发现存在一定程度的9,10-蒽醌污染,且超标率较高。其中,黑茶和红茶的检测结果中位数为35.1 μg/kg和25.9 μg/kg,污染程度明显高于乌龙茶和绿茶。结论该方法具有仪器自动化程度高,前处理快速简单,溶剂消耗少,灵敏度高,定性定量准确等特点,适合大批量茶叶样品中9,10-蒽醌的快速筛查检测。

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关键词 ：基质分散固相萃取, 在线凝胶渗透色谱-气相色谱-串联质谱, 9,10-蒽醌, 茶叶

Abstract：Objective To establish a rapid method for the determination of 9,10-anthraquinone in tea by quick, easy, cheap, effective, rugged and safe (QuEChERS) method coupled with on-line gel permeation chromatography- gas chromatography-mass/mass spectrometry (GPC-GC-MS/MS), to detect the residue of 9,10-anthraquinone in tea sold in Hunan Province, and to analyze the detection results. Methods 9,10-anthraquinone was extracted with 1:1 cyclohexane-ethyl acetate, purified by QuEChERS method, analyzed and detected by on-line GPC-GC-MS/MS. The quantification was accomplished by internal standard method with d8-anthraquinone as the internal standard. Results 9,10-anthraquinone in tea showed a good linear relationship with the peak area in the concentration range of 1-100 μg/L. The linear equation was y =0.0311x-0.0023, and the correlation coefficient was 0.9997. The limit of detection (LOD) was 2 μg/kg, and the limit of quantitation (LOQ) 5 μg/kg. The recoveries ranged from 75.8% to 98.4%, with the relative standard deviation (RSD) of 2.6%-6.6% (n=6). It was found that there was a certain degree of 9,10-anthraquinone pollution in tea sold in 14 cities in Hunan Province, and the exceeding standard rate was high. Among them, the median values of dark tea and black tea were 35.1 μg/kg and 25.9 μg/kg, respectively, and their pollution degrees were significantly higher than those of oolong tea and green tea. Conclusion The method has the characteristics of high automation, fast and simple pretreatment, low solvent consumption, high sensitivity and qualitative and quantitative accuracy. It is suitable for the rapid screening of 9,10-anthraquinone in large quantities of tea samples.

Key words： QuEChERS on-line gel permeation chromatography-gas chromatography-mass/mass spectrometry 9,10-anthraquinone tea

收稿日期: 2022-03-29

R155.3

基金资助:湖南省自然科学基金项目(2021JJ70085)

通讯作者: 刘先军,E-mail: 332499047@qq.com。

作者简介: 李谭瑶(1984-),女,湖南益阳人,主管技师,主要从事食品安全检测工作。

引用本文:

李谭瑶, 冯家力, 曾栋, 陈东洋, 卢岚, 刘先军. 基质分散固相萃取联合在线凝胶渗透色谱-气相色谱-串联质谱法测定湖南省市售茶叶中9,10-蒽醌的含量[J]. 实用预防医学, 2022, 29(10): 1187-1190. LI Tan-yao, FENG Jia-li, ZENG Dong, CHEN Dong-yang, LU Lan, LIU Xian-jun. Application of QuEChERS method coupled with on-line GPC-GC-MS/MS for determination of 9,10-anthraquinone in tea sold in Hunan Province. , 2022, 29(10): 1187-1190.

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https://www.syyfyx.com/CN/10.3969/j.issn.1006-3110.2022.10.008 或 https://www.syyfyx.com/CN/Y2022/V29/I10/1187

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