超高效液相色谱-串联质谱法检测绿茶中16种农药残留

doi:10.13305/j.cnki.jts.20220416.004

摘要/Abstract

摘要： 建立了超高效液相色谱-串联质谱（UPLC-MS/MS）同时检测绿茶中16种农药残留的分析方法。采用1%甲酸乙腈提取绿茶样品中的目标农药,经TPT-SPE柱净化,在电喷雾正离子源（ESI⁺）模式下电离,质谱多反应监测模式（MRM）对目标母离子和子离子进行扫描测定。通过对样品提取、净化以及色谱条件优化,目标农药浓度范围在0.005~1.000 mg·kg^-1线性良好,相关系数R²>0.992 6;在0.010、0.050、0.100 mg·kg^-1和1.000 mg·kg^-1 4个添加水平下,平均回收率在74.0%~105.4%,相对标准偏差（RSD）<20.0%;方法的定量限为10~50 μg·kg^-1。该方法分析速度快,灵敏度高,各项技术指标均符合国内外相关法规标准,可满足绿茶中多种农药残留同时检测的要求。

关键词: 农药多残留分析, 超高效液相色谱-串联质谱, TPT-SPE柱净化, 绿茶

Abstract: An analytical method was developed for the simultaneous determination of 16 pesticide residues in green tea by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target pesticides in tea samples were extracted by acetonitrile with 1% formic acid, cleaned up by a TPT-SPE column, ionized in electrospray positive ionization source (ESI⁺) mode, and scanned for determination of the target parent and daughter ions by mass spectrometry in multiple reaction monitoring mode (MRM). The results show that the target pesticides were linear in the range of 0.005-1.000 mg·kg^-1 with the correlation coefficient R²>0.992 6. The average recoveries ranged from 74.0% to 105.4% at the four spiked levels of 0.010, 0.050, 0.100、1.000 mg·kg^-1, and the relative standard deviations (RSD) were <20.0%. The limits of quantification were 10-50 μg·kg^-1. The method is fast and sensitive, and the technical parameters are in accordance with the relevant domestic and international regulations and standards. And it can meet the requirements of simultaneous determination of various pesticide residues in green tea.

Key words: multi-residue of pesticides analysis, UPLC-MS/MS, TPT-SPE column clean, green tea

中图分类号:

S571.1

李自强, 杨梅, 张新忠, 罗逢健, 周利, 楼正云, 孙荷芝, 王新茹, 陈宗懋. 超高效液相色谱-串联质谱法检测绿茶中16种农药残留[J]. 茶叶科学, 2022, 42(4): 537-548. doi: 10.13305/j.cnki.jts.20220416.004.

LI Ziqiang, YANG Mei, ZHANG Xinzhong, LUO Fengjian, ZHOU Li, LOU Zhengyun, SUN Hezhi, WANG Xinru, CHEN Zongmao. Residue Determination of Sixteen Pesticides in Green Tea by UPLC-MS/MS[J]. Journal of Tea Science, 2022, 42(4): 537-548. doi: 10.13305/j.cnki.jts.20220416.004.

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