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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. 分析化学, 2017, 45(11): 1669-1677. doi:  10.11895/j.issn.0253-3820.170224 [复制]

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. Chinese Journal of Analytical Chemistry, 2017, 45(11): 1669-1677. doi: 10.11895/j.issn.0253-3820.170224 [复制]

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

通讯作者:  周志钦, fruitnutri@swu.edu.cn

收稿日期: 2017-04-12

接受日期: 2017-08-12

出版日期: 2017-11-20

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

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

Corresponding author:  ZHOU Zhi-Qin, fruitnutri@swu.edu.cn

Received Date:  2017-04-12

Accepted Date:  2017-08-12

Published Date:  2017-11-20

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:   纳米多孔碳, 柑橘皮渣, 气相色谱, 有机磷农药, 净化
Key words:   Porous carbon nanoparticles, Citrus waste, Gas chromatography, Organophosphorus pesticides, Clean-up
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目录

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

任科宇, 张文林, 曹淑瑞, 郗存显, 王国民, 周志钦

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