超高效液相色谱-串联质谱法同时测定茶鲜叶中79种农药残留

doi:10.13305/j.cnki.jts.2023.02.004

摘要/Abstract

摘要： 建立以超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定茶鲜叶中79种农药残留量的分析方法。以乙腈为提取剂,茶鲜叶样品经高速破壁均质后加入NaCl盐析,离心取上清液经无水硫酸镁、C₁₈、PSA和GCB分散固相萃取净化后上机,多反应监测模式扫描,分段时间窗口采集数据,外标法定量。结果显示,79种目标化合物在0.001~0.400 mg·L^-1质量浓度范围内线性良好,相关系数（R²）为0.990 6~0.999 9,在0.01、0.03、0.05、0.10 mg·kg^-1和0.20 mg·kg^-1等5个添加水平下的平均回收率为70.7%~119.0%,相对标准偏差（RSD）为0.1%~19.8%,方法定量限为0.01~0.05 mg·kg^-1。该方法灵敏度高、准确性好、分析速度快,适用于茶鲜叶中79种农药残留的检测。

关键词: 茶鲜叶, 超高效液相色谱-串联质谱法, 农药残留, 回收率

Abstract: A method for simultaneous determination of 79 pesticides residues in fresh tea leaves by ultra-high performance liquid chromatography-mass spectrometry (UPLC-MS/MS) was establish in this study. The fresh tea leaves were ground by high-speed wall breaking and then extracted by acetonitrile solution with NaCl. The liquid supernatant was centrifuged and purified by solid phase extraction of anhydrous magnesium sulfate, C₁₈, PSA and GCB. The scheduled multiple reaction monitoring mode (sMRM) was used for scanning and determination, and quantitative by external standard method. The results show that the 79 target compounds exhibited good linearity within the concentration range of 0.001~0.400 mg·L^-1 with a correlation coefficient (R²) of 0.990 6 to 0.999 9. The average recoveries at 5 spiked levels (0.01, 0.03, 0.05, 0.10, 0.20 mg·kg^-1) ranged from 70.7% to 119.0%, with the relative standard deviations (RSDs) ranging from 0.1% to 19.8%, and the limits of quantitation (LOQ) for the 79 pesticides ranging from 0.01 mg·kg^-1 to 0.05 mg·kg^-1. The proposed method is high sensitivity, good accuracy and quick, which is suitable for determination of 79 pesticides residues in fresh tea leaves.

Key words: fresh tea leaves, UPLC-MS/MS, pesticide residues, recovery

中图分类号:

S571.1

潘瑛洁, 孟祥河, 钱园凤, 宁建美, 王月圆, 刘齐铭, 唐仕琴, 徐晓安, 叶沁. 超高效液相色谱-串联质谱法同时测定茶鲜叶中79种农药残留[J]. 茶叶科学, 2023, 43(2): 250-262. doi: 10.13305/j.cnki.jts.2023.02.004.

PAN Yingjie, MENG Xianghe, QIAN Yuanfeng, NING Jianmei, WANG Yueyuan, LIU Qiming, TANG Shiqin, XU Xiaoan, YE Qin. Simultaneous Determination of 79 Pesticides Residues in Fresh Tea Leaves by Ultra-high Performance Liquid Chromatography-mass Spectrometry[J]. Journal of Tea Science, 2023, 43(2): 250-262. doi: 10.13305/j.cnki.jts.2023.02.004.

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