烯丙基氧七元瓜环固相微萃取纤维联用气相色谱同时检测蔬菜中的有机氯与有机磷农药残留

张凌雪; 罗玉洁; 马培舰; 姚键梅; 卫刚; 董南

doi:doi：10.3969/j.issn.1004-4957.2019.11.009

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烯丙基氧七元瓜环固相微萃取纤维联用气相色谱同时检测蔬菜中的有机氯与有机磷农药残留

- 烯丙基氧七元瓜环固相微萃取纤维联用气相色谱同时检测蔬菜中的有机氯与有机磷农药残留
- Determination of Organochlorine and Organophosphorus Pesticide Residues in Vegetables by Gas Chromatography Coupled with Solid phase Microextraction Fiber Based on Allyl-o-cucurbit［7］uril
- 分析测试学报 2019年38卷第11期页码：1340-1346
- 作者机构：
  
  1. 贵州大学化学与化工学院
  2. 贵州省草地技术试验推广站
  3. Commonwealth Scientific and Industrial Research Organization
  4. Manufacturing
  5. 贵州大学贵州省大环化学及超分子化学重点实验室
- 作者简介：
- 基金信息：
  
  国家自然科学基金(21665005);教育部“春晖计划”资助项目(Z2017006)
- DOI：doi：10.3969/j.issn.1004-4957.2019.11.009
  中图分类号：
- 纸质出版：2019
- 稿件说明：
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张凌雪, 罗玉洁, 马培舰, 姚键梅, 卫刚, 董南. 烯丙基氧七元瓜环固相微萃取纤维联用气相色谱同时检测蔬菜中的有机氯与有机磷农药残留[J]. 分析测试学报, 2019,38(11):1340-1346.

张凌雪, 罗玉洁, 马培舰, 姚键梅, 卫刚, 董南. Determination of Organochlorine and Organophosphorus Pesticide Residues in Vegetables by Gas Chromatography Coupled with Solid phase Microextraction Fiber Based on Allyl-o-cucurbit［7］uril[J]. 2019, 38(11): 1340-1346.
张凌雪, 罗玉洁, 马培舰, 姚键梅, 卫刚, 董南. 烯丙基氧七元瓜环固相微萃取纤维联用气相色谱同时检测蔬菜中的有机氯与有机磷农药残留[J]. 分析测试学报, 2019,38(11):1340-1346. DOI： doi：10.3969/j.issn.1004-4957.2019.11.009.

张凌雪, 罗玉洁, 马培舰, 姚键梅, 卫刚, 董南. Determination of Organochlorine and Organophosphorus Pesticide Residues in Vegetables by Gas Chromatography Coupled with Solid phase Microextraction Fiber Based on Allyl-o-cucurbit［7］uril[J]. 2019, 38(11): 1340-1346. DOI： doi：10.3969/j.issn.1004-4957.2019.11.009.

摘要

以烯丙基氧七元瓜环(Q7-OCH2CH‖CH2)和端羟基聚二甲基硅氧烷(OH-PDMS)为固定相，γ 甲基丙烯酰氧基丙基三甲氧基硅烷(KH570)为偶联试剂，利用溶胶-凝胶方法和自由基交联技术首次制备了PDMS/Q7-OCH2CH‖CH2涂层的固相微萃取纤维，建立了PDMS/Q7-OCH2CH‖CH2 SPME纤维-气相色谱(GC)/氢火焰离子化检测器(FID)对蔬菜中10种有机氯、有机磷农药残留同时检测的分析方法。结果显示，10种农药的检出限(LOD)为0.01~0.08 mg/kg，定量下限(LOQ)为0.03~0.26 mg/kg，富集倍数为14~67倍。低、中、高3个水平下的平均回收率(n=3)为61.3%~120%，日内及日间精密度(RSD)为4.6%~9.9%(n=5

50 mg/kg)。方法灵敏、简便，可满足蔬菜中有机氯、有机磷农残同时测定的要求。

Abstract

A gas chromatography with flame ionization detector(GC/FID) was developed for the determination of ten organochlorine and organophosphorus pesticide residues in vegetable samples based on a polydimethylsiloxane(PDMS)/allyl o cucurbit［7］uril(Q7-OCH2CH‖CH2) coated solid phase microextraction(SPME) fiber.The PDMS/Q7-OCH2CH‖CH2 coated SPME fiber was fabricated with Q7-OCH2CH‖CH2 and hydroxyl terminated polydimethylsiloxane(OH-PDMS) as stationary phases and γ-methacryloxypropyltrimethoxylsilane(KH570) as bridge reagent by sol-gel method and cross-linking technique.The limits of detection of the developed method were in the range of 0.01-0.08 mg/kg for the target pesticide residues

and the limits of quantitation ranged from 0.03 mg/kg to 0.26 mg/kg with an enrichment factor of 14-67 fold.The mean recoveries(n=3) at low

medium and high three spiked levels ranged from 61.3%to 120%

with intra percision and inter precision both in the range of 46%-99%(n=5

spiked 50 mg/kg).The proposed method was simple and sensitive

and was suitable for the simultaneous analysis of organochlorine and organophosphorus pesticide residues in vegetables.

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