GC-MS法测定蔬菜中3，5，6-三氯-2羟基吡啶

doi:10.7506/spkx1002-6630-201024059

食品科学 ›› 2010, Vol. 31 ›› Issue (24): 277-280.doi: 10.7506/spkx1002-6630-201024059

GC-MS法测定蔬菜中3，5，6-三氯-2羟基吡啶

谢娟^1,2，王颜红1,*，王世成¹，张红¹，王莹¹，王姗姗¹

1.中国科学院沈阳应用生态研究所
2.中国科学院研究生院

收稿日期:2010-02-03 修回日期:2010-10-26 出版日期:2010-12-25 发布日期:2010-12-29
通讯作者: 王颜红 E-mail:wangyh@iae.ac.cn
基金资助:
财政部社会公益研究项目(2007-10)；沈阳市科技支撑计划项目(1081197-3-00)

Determination of 3, 5, 6-Trichloro-2-pyridinol in Vegetables by Gas Chromatography-Mass Spectrometry

XIE Juan1,2，WANG Yan-hong1,*，WANG Shi-cheng1，ZHANG Hong1，WANG Ying1，WANG Shan-shan1

1. Institute of Applied Ecology, Chinese Academy of Sciences, Shenyang 110016, China ；
2. Graduate University of Chinese Academy of Sciences, Beijing 100049, China

Received:2010-02-03 Revised:2010-10-26 Online:2010-12-25 Published:2010-12-29
Contact: WANG Yan-hong E-mail:wangyh@iae.ac.cn

摘要/Abstract

摘要：

建立蔬菜中毒死蜱代谢物3,5,6- 三氯-2 羟基吡啶(3,5,6-trichloro-2-pyridinol，TCP)的气相色谱- 质谱检测方法。样品经丙酮提取，正己烷去除杂质，二氯甲烷反萃取，过无水硫酸钠去除水分，浓缩后乙酸乙酯溶解，再用N-(特丁基二甲基硅烷基)-N- 甲基三氟乙酰胺(MTBSTFA)衍生，正己烷定容，经气相色谱- 质谱检测，外标法定量。方法的检出限为8.3μg/kg，加标回收率为70.4%～107.6%，RSD 为4.3%～8.7%。在5～500μg/L 的范围内线性范围良好，相关系数大于0.99。该方法通用性强，灵敏度高，可用于蔬菜中TCP 的检测。

关键词: 气相色谱- 质谱, 3,5,6- 三氯-2 羟基吡啶, 蔬菜

Abstract:

A gas chromatography-mass spectrometry (GC-MS) method was established for the determination of 3,5,6- trichloro-2-pyridinol (TCP), a kind of metabolite of chlorpyrifos in vegetables. The sample was extracted by acetone, and the extract was purified using hexane and DCM. The water was removed with anhydrous sodium sulfate. After condensation, the extract was dissolved into 1 mL of ethyl acetate and then derivatized with N-(tert-butyldimethylsilyl)-methyltrifluoroacetamide (MTBSTFA), and finally the volume was adjusted to 1 mL using hexane. The analyte was detected by GC-MS, and an external standard method was used for quantifying TCP. The limit of detection was 8.3μg/kg, and the recovery rates of spiked sample were in the range of 70.4% － 107.6% with relative standard deviation of 4.3% － 8.7%. An excellent linear relationship was achieved in the range of 5－500μg/L with correlation coefficients over 0.99. This method is characteristics of accuracy, easy operation and can be applied for determining TCP in vegetables.

Key words: gas chromatography-mass spectrometry(GC-MS), 3,5,6-trichloro-2-pyridinol, vegetables

中图分类号:

O657.73

谢娟1,2，王颜红1,*，王世成1，张红1，王莹1，王姗姗1. GC-MS法测定蔬菜中3，5，6-三氯-2羟基吡啶[J]. 食品科学, 2010, 31(24): 277-280.

XIE Juan1,2，WANG Yan-hong1,*，WANG Shi-cheng1，ZHANG Hong1，WANG Ying1，WANG Shan-shan1. Determination of 3, 5, 6-Trichloro-2-pyridinol in Vegetables by Gas Chromatography-Mass Spectrometry[J]. FOOD SCIENCE, 2010, 31(24): 277-280.

[1]	李凯龙，陈同强，徐文泱，李涛，王亮亮，王芳，孙桂芳. 超声辅助浊点萃取-液相色谱-串联质谱法测定蔬菜中天然VK同系物[J]. 食品科学, 2021, 42(8): 214-220.
[2]	鲍伟，韩姣姣，张旨轩，芦晨阳，周君，明庭红，李晔，苏秀榕. 基于高通量测序技术对浙江传统发酵蔬菜微生物多样性的解析[J]. 食品科学, 2021, 42(6): 178-185.
[3]	高霞，陈辉，谭敏，李玉秀，何泓霖. 气相色谱-负化学源电离-质谱法测定蔬菜中氟虫腈及其代谢物残留[J]. 食品科学, 2021, 42(14): 333-338.
[4]	徐尉力，付壮，王旭，赵悦，王晨兆，马佳骏，王志兵. 沉积固化离子液体均相液液微萃取-高效液相色谱法测定蔬菜中的苯脲类农药残留[J]. 食品科学, 2020, 41(4): 248-255.
[5]	司阔林，徐捐捐，岳田利，袁亚宏，郭春锋. 布氏乳杆菌产γ-氨基丁酸发酵条件的优化[J]. 食品科学, 2020, 41(2): 87-93.
[6]	康建依，洪洁，高逸，杨悦，陈孟，易欣欣，高秀芝. 山西地方自然发酵蔬菜发酵过程中细菌多样性分析[J]. 食品科学, 2019, 40(10): 106-111.
[7]	谢思思，卢俊文，李蓉，张宪臣，张朋杰，容裕棠，陈丽斯，谢丽芳. QuEChERS-气相色谱-串联质谱法测定蔬菜中35 种多氯联苯[J]. 食品科学, 2018, 39(6): 307-314.
[8]	郑秋丽，王清，高丽朴，王云香，史君彦，左进华. 蔬菜保鲜包装技术的研究进展[J]. 食品科学, 2018, 39(3): 317-323.
[9]	高媛，王蒙，王瑶，吕晓玲，冯晓元. 蔬菜及其制品中不同形态酚酸成分分析[J]. 食品科学, 2018, 39(24): 189-194.
[10]	朱瑞欣，兰晓芳，范志红，王琳琳. 5种蔬菜对米饭餐后血糖反应的影响[J]. 食品科学, 2018, 39(19): 207-211.
[11]	吴延灿，蒋冰心，施艳红，戚传勇，操海群，唐俊，商鲁宁，苏漪玲. QuPPe-超高效液相色谱-串联质谱法测定蔬菜中呋虫胺及其代谢物残留[J]. 食品科学, 2018, 39(18): 262-266.
[12]	叶陵，李勇，王蓉蓉，刘成国，蒋立文，邓放明，周辉. 我国传统发酵蔬菜中乳酸菌多样性的研究进展[J]. 食品科学, 2018, 39(15): 296-301.
[13]	王坦，刘福光，董茂锋，王伟民，陈珊珊，戚亚梅，郭林宇，宋卫国. 中欧蔬菜农药残留检测方法差异及应对[J]. 食品科学, 2018, 39(13): 317-323.
[14]	潘城，胡朝阳，吴凌，谢勇，黄永辉. 高效液相色谱法测定蔬菜中异菌脲残留量的不确定度分析[J]. 食品科学, 2017, 38(24): 235-240.
[15]	王建华，葛敏敏，张慧丽，林洪，汤志旭，李立. QuEChERS法-液相色谱-串联质谱法测定蔬菜中7 种农药及其代谢物的残留量[J]. 食品科学, 2017, 38(20): 235-241.

GC-MS法测定蔬菜中3，5，6-三氯-2羟基吡啶

Determination of 3, 5, 6-Trichloro-2-pyridinol in Vegetables by Gas Chromatography-Mass Spectrometry

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价