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

发布时间：2018-05-15 11:26

本文选题：纳米多孔碳 + 柑橘皮渣　；参考：《分析化学》2017年11期

【摘要】：以废弃柑橘皮渣为碳源,通过Zn Cl2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(R20.99),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。
[Abstract]:Using waste citrus peel residue as carbon source, nanometer porous carbon material was prepared by high temperature calcination after activation of Zn Cl2. A method for the determination of organophosphorus pesticide residues in fruits and vegetables by gas chromatography was established by using dispersed solid phase extraction (SPE) as adsorbent. Scanning Electron Microscopy (SEM), SEM, FTIR, Raman spectra and nitrogen adsorption analysis show that NPCs are amorphous porous carbon materials with a pore size of 0.15 nm, specific surface area of 1243 m2 / g and pore volume of 1.28 cm ~ (3 / g), respectively. Taking 14 organophosphorus pesticides in fruits and vegetables as the analytical object, the amount of adsorbent and the purification time were investigated. The NPC was compared with the commercial materials N- propyl ethylenediamine, octadecyl silica gel bonded phase C18) and graphitized carbon black GCBs. The results showed that the optimal usage of min.NPC was 0. 01 g, and the cost of purification time was 2 min.NPC, which was much lower than that of C18 min.NPC and GCB. because of its abundant pore structure, the purification effect of NPCs was significantly better than that of three commercial materials. Under the optimum conditions, the linear relationship of 14 organophosphorus pesticides in the range of 0.02 ~ 1.0 mg/L is good, the detection limit is 0.63 ~ 5.30 渭 g/kg.3, the average recovery is 71.3 ~ 114.7and the relative standard deviation (RSD) is 0.912.9. The method is simple, rapid and low cost, and has a broad application prospect in fruit and vegetable sample pretreatment.
【作者单位】：西南大学园艺园林学院;南方山地园艺学教育部重点实验室;重庆出入境检验检疫局;
【基金】：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) 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
【分类号】：O657.71;TS255.7

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