固相萃取和分散固相净化-串联质谱测定茶鲜叶和干茶中的农药残留

doi:10.13305/j.cnki.jts.2020.03.010

摘要/Abstract

摘要： 建立了茶鲜叶和干茶中9种农药的残留分析方法。样品中的残留农药经乙腈提取,Florisil/GCB固相萃取柱和PSA/GCB分散固相联合净化,超高效液相色谱串联质谱（UPLC-MS/MS）和气相色谱质谱联用（GC-MS）测定。在0.005~1.000 mg·kg^-1的添加水平下,目标农药在鲜叶和干茶中的平均回收率在70.3%~103.9%,相对标准偏差（RSD）<20.0%。在0.005~2.000 mg·kg^-1浓度范围,目标农药在鲜叶和干茶基质中的线性关系良好,r>0.995 4。定量限（LOQ）为0.005 mg·kg^-1。实际样品检测结果表明,该方法灵敏度高,重现性好,能够满足农药多残留检测的要求。

关键词: 农药多残留, 超高效液相色谱串联质谱, 气相色谱质谱联用, 茶, 固相萃取, 分散固相净化

Abstract: A method for the determination of 9 pesticide residues in fresh and dry tea was established. Residual pesticides in samples were extracted by acetonitrile, purified by Florisil/GCB solid phase extraction column, followed by absorbent of PSA and GCB as dispersed solid phase, and determined by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and gas chromatography-mass spectrometry (GC-MS). In the spiked range of 0.005-1.000 mg·kg^-1, the average recoveries of target pesticides in fresh leaves and dried tea were 70.3%-103.9%, and the relative standard deviations (RSD) were less than 20%. In the range of 0.005-2.000 mg·kg^-1, the linear relationship of target pesticides in fresh leaves and dry tea matrix was good, with r>0.995 4. The limit of quantity (LOQ) was 0.005 mg·kg^-1. The test results of actual samples showed that the method was highly sensitive and reproducible, and can meet the requirements of multi-residue detection.

Key words: multi-residue of pesticides, UPLC-MS/MS, GC-MS, tea, solid phase extraction, dispersive solid-phase extraction

中图分类号:

S571.1
S482

杨洁, 周利, 余焕, 孙荷芝, 王新茹, 张新忠, 杨梅, 陈宗懋, 罗逢健. 固相萃取和分散固相净化-串联质谱测定茶鲜叶和干茶中的农药残留[J]. 茶叶科学, 2020, 40(3): 397-406. doi: 10.13305/j.cnki.jts.2020.03.010.

YANG Jie, ZHOU Li, YU Huan, SUN Hezhi, WANG Xinru, ZHANG Xinzhong, YANG Mei, CHEN Zongmao, LUO Fengjian. Determination of Pesticide Residue in Fresh Tea Leaves and Dry Tea by Solid Extraction and Dispersive Solid Extraction Cleanup Coupled with Tandem Mass Spectrum[J]. Journal of Tea Science, 2020, 40(3): 397-406. doi: 10.13305/j.cnki.jts.2020.03.010.

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