加速溶剂萃取-固相萃取净化-气相色谱-串联质谱法检测茶叶中9种拟除虫菊酯类农药残留

引用本文: 黄微, 李娜, 徐瑞晗, 李婷, 李崇勇. 加速溶剂萃取-固相萃取净化-气相色谱-串联质谱法检测茶叶中9种拟除虫菊酯类农药残留[J]. 色谱, 2018, 36(12): 1303-1310. doi: 10.3724/SP.J.1123.2018.09019 shu

Citation: HUANG Wei, LI Na, XU Ruihan, LI Ting, LI Chongyong. Determination of nine pyrethroid pesticide residues in tea by gas chromatography-tandem mass spectrometry combined with accelerated solvent extraction and solid phase extraction[J]. Chinese Journal of Chromatography, 2018, 36(12): 1303-1310. doi: 10.3724/SP.J.1123.2018.09019 shu

加速溶剂萃取-固相萃取净化-气相色谱-串联质谱法检测茶叶中9种拟除虫菊酯类农药残留

黄微 ^1, ,
李娜 ^1, ,
徐瑞晗 ^2, ,
李婷 ^1, ,
李崇勇 ^1,

1.
汉中市食品药品检验检测中心, 陕西汉中 723000;
2.
汉中市动物卫生监督所, 陕西汉中 723000

摘要: 建立了加速溶剂萃取（ASE）-固相萃取净化（SPE）-气相色谱-串联质谱（GC-MS/MS）同时测定茶叶中9种拟除虫菊酯类农药残留的方法。ASE萃取溶剂为丙酮-正己烷（1：1，v/v），萃取温度为100℃，萃取压力为10 MPa，加热时间为3 min，静态萃取时间为5 min，循环1次，冲洗体积为40%萃取池体积，氮气吹扫100 s。萃取结束后用Cleanert TPT固相萃取柱净化，净化液浓缩定容后，采用GC-MS/MS测定，外标法定量。9种拟除虫菊酯类农药在2~1000 μg/L范围内呈现良好的线性关系，相关系数（r²）均大于0.99，方法检出限为0.2~4.5 μg/kg，定量限为0.8~15.0 μg/kg。在绿茶、红茶空白基质中做加标回收试验，添加水平为0.02、0.1、0.4 mg/kg以及定量限水平，得到的平均回收率为69.87%~110.0%，相对标准偏差（RSD）为0.7%~11.2%。该方法背景干扰低、灵敏度高、重现性好、回收率稳定，适用于茶叶中拟除虫菊酯类农药残留量的检测。

关键词:

English

Determination of nine pyrethroid pesticide residues in tea by gas chromatography-tandem mass spectrometry combined with accelerated solvent extraction and solid phase extraction

1.
Hanzhong Control and Testing Center for Food and Drug, Hanzhong 723000, China;
2.
Hanzhong Animal Hygienie Supervision Institute, Hanzhong 723000, China
Received Date: 11 September 2018

Abstract: A method has been developed for the simultaneous detection of nine pyrethroid pesticide residues in tea by gas chromatography-tandem mass spectrometry (GC-MS/MS) combined with accelerated solvent extraction (ASE) and solid-phase extraction (SPE). The pesticide residues in tea were extracted using acetone/n-hexane (1:1, v/v) for 5 min at 100℃ before preheating the extraction pool for 3 min, under extractive pressure of 10 MPa for one cycle. After extraction, the extraction pool was washed with acetone/n-hexane (1:1, v/v) having volume of 40% of the pool volume, followed by purging for 100 s with nitrogen. The extract was purified by a Cleanert TPT solid-phase extraction column. After purification, the target compounds were detected by GC-MS/MS and quantified by the external standard method. Under the optimized conditions, good linearities were obtained for the nine pyrethroid pesticides in the range of 2-1000 μg/L, with correlation coefficients exceeding 0.99. The limits of detection (LODs) were 0.2-4.5 μg/kg and the limits of quantitation (LOQs) were 0.8-15.0 μg/kg. At four spiked levels (0.02, 0.1, 0.4 mg/kg, and the LOQ level) in green tea and black tea, the recoveries of all the pesticides were between 69.87% and 110.0%, with relative standard deviations (RSDs) varying from 0.7% to 11.2%. This method effectively reduces the matrix interference and shows high sensitivity, good reproducibility, and stable recovery, and can thus be used for the detection of pyrethroid pesticide residues in tea.

Key words:

gas chromatography-tandem mass spectrometry (GC-MS/MS)
/ accelerated solvent extraction (ASE)
/ pyrethroid pesticides
/ tea

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加速溶剂萃取-固相萃取净化-气相色谱-串联质谱法检测茶叶中9种拟除虫菊酯类农药残留

English

Determination of nine pyrethroid pesticide residues in tea by gas chromatography-tandem mass spectrometry combined with accelerated solvent extraction and solid phase extraction

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加速溶剂萃取-固相萃取净化-气相色谱-串联质谱法检测茶叶中9种拟除虫菊酯类农药残留

English

Determination of nine pyrethroid pesticide residues in tea by gas chromatography-tandem mass spectrometry combined with accelerated solvent extraction and solid phase extraction

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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