基于柑橘皮渣纳米多孔碳分散固相萃取-气相色谱法测定果蔬中14种有机磷农药残留

引用本文: 任科宇, 张文林, 曹淑瑞, 郗存显, 王国民, 周志钦. 基于柑橘皮渣纳米多孔碳分散固相萃取-气相色谱法测定果蔬中14种有机磷农药残留[J]. 分析化学, 2017, 45(11): 1669-1677. doi: 10.11895/j.issn.0253-3820.170224 shu

Citation: REN Ke-Yu, ZHANG Wen-Lin, CAO Shu-Rui, XI Cun-Xian, WANG Guo-Min, ZHOU Zhi-Qin. Determination of Organophosphorus Pesticide Residues in Fruits and Vegetables Using Porous Carbon Nanoparticles Based on Citrus Compose[J]. Chinese Journal of Analytical Chemistry, 2017, 45(11): 1669-1677. doi: 10.11895/j.issn.0253-3820.170224 shu

基于柑橘皮渣纳米多孔碳分散固相萃取-气相色谱法测定果蔬中14种有机磷农药残留

1.
西南大学园艺园林学院, 重庆 400716;
2.
南方山地园艺学教育部重点实验室, 重庆 400715;
3.
重庆出入境检验检疫局, 重庆 400020
基金项目:
本文系重庆市现代农业特色产业技术体系：晚熟柑橘产业技术体系（No.20174-4）和2016食用农产品特征性营养组成识别与验证评估专项（No.GJFP201601501，No.GJFP201601503）资助。

摘要: 以废弃柑橘皮渣为碳源，通过ZnCl₂活化后高温煅烧制备了纳米多孔碳材料（NPC），将其作为吸附剂，建立了分散固相萃取净化、气相色谱法测定果蔬中有机磷农药残留的方法。扫描电子显微镜（SEM）、X射线衍射（XRD）、傅立叶红外光谱（FT-IR）、拉曼光谱及氮气吸附分析（BET）等表征显示，NPC是无定形的多孔碳材料，孔径大小为0~15 nm，比表面积和孔体积分别为1243 m²/g和1.28 cm³/g。以果蔬中14种有机磷类农药为分析对象，考察了吸附剂的用量和净化时间，并将NPC与商业化材料N-丙基乙二胺（PSA）、十八烷基硅胶键合相（C₁₈）和石墨化碳黑（GCB）进行了对比。结果表明，NPC最佳使用量为0.01 g，净化时间只需2 min。NPC成本远低于C₁₈、PSA和GCB，因具有丰富的孔道结构，NPC净化效果显著优于3种商业化材料。在最优条件下，14种有机磷农药在0.02-1.0 mg/L范围内的线性关系良好（R²>0.99），检出限（S/N=3）为0.63-5.30μg/kg。3个添加水平下的平均回收率为71.3%-114.7%，相对标准偏差（RSD）为0.9%-12.9%。本方法操作简便、快速、成本低，在果蔬样品前处理中具有广阔的应用前景。

关键词:

English

Determination of Organophosphorus Pesticide Residues in Fruits and Vegetables Using Porous Carbon Nanoparticles Based on Citrus Compose

1.
College of Horticulture and Landscape Architecture, Southwest University, Chongqing 400716, China;
2.
Key Laboratory of Horticulture Science for Southern Mountainous Regions, Ministry of Education, Chongqing 400715, China;
3.
Chongqing Entry-exit Inspection and Quarantine Bureau, Chongqing 400020 China
Received Date: 12 April 2017
Revised Date: 12 August 2017

Abstract: Porous carbon nanoparticles (NPC) were prepared by ZnCl₂ activation and carbonization using citrus waste as carbon source. A sample pretreatment method with NPC as dispersive solid phase extraction (d-SPE) absorbent was established for the determination of organophosphorus pesticides in fruits and vegetables by gas chromatography. The NPC was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), FT-IR spectra, Raman spectroscopy, Brunauer, Emmett and Teller surface area (BET). Those results showed that the NPC was an amorphous porous carbon material with pore size in the range of 0-15 nm. Its specific surface area and pore volume were 1243 m²/g and 1.28 cm³/g, respectively. The analysis conditions, including the amount and clean up time of adsorbent, were optimized by analysis of 14 kinds of oranophosphorus pesticides in fruits and vegetables with gas chromatography-flame photometric determination(GC-FPD). Moreover, the comparison for NPC with commercial materials of PSA, C₁₈ and GCB was investigated in this study. The results indicated that the purification time was only 2 min using 0.01 g NPC. The cost of NPC was about 25% of C₁₈, 21% of PSA and 16% of GCB. Because of the porous structure of NPC, the purification efficiency was significantly higher than the three commercial materials mentioned above. Under the optimum conditions, the calibration curves of the 14 organophosphorus pesticides were linear in the range of 0.02-1.00 mg/L with good correlation coefficients (R²>0.99) and detection limits (S/N=3) of 0.63-5.30 μg/kg. The recoveries of the pesticides at three spiked levels ranged from 71.3% to 114.7% with the relative standard deviations (RSDs) of 0.9%-12.9%. The method is simple, rapid, sensitive, and low cost, and can satisfy the requirements of detection of organophosphorus pesticide residues in fruits and vegetables, displaying a good application prospect.

Key words:

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1.
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基于柑橘皮渣纳米多孔碳分散固相萃取-气相色谱法测定果蔬中14种有机磷农药残留

English

Determination of Organophosphorus Pesticide Residues in Fruits and Vegetables Using Porous Carbon Nanoparticles Based on Citrus Compose

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

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

基于柑橘皮渣纳米多孔碳分散固相萃取-气相色谱法测定果蔬中14种有机磷农药残留

English

Determination of Organophosphorus Pesticide Residues in Fruits and Vegetables Using Porous Carbon Nanoparticles Based on Citrus Compose

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

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs