發(fā)布時(shí)間：2018-05-15 11:26

  本文選題：納米多孔碳 + 柑橘皮渣　； 參考：《分析化學(xué)》2017年11期

【摘要】：以廢棄柑橘皮渣為碳源,通過Zn Cl2活化后高溫煅燒制備了納米多孔碳材料(NPC),將其作為吸附劑,建立了分散固相萃取凈化、氣相色譜法測(cè)定果蔬中有機(jī)磷農(nóng)藥殘留的方法。掃描電子顯微鏡(SEM)、X射線衍射(XRD)、傅立葉紅外光譜(FT-IR)、拉曼光譜及氮?dú)馕椒治?BET)等表征顯示,NPC是無定形的多孔碳材料,孔徑大小為0~15 nm,比表面積和孔體積分別為1243 m2/g和1.28 cm3/g。以果蔬中14種有機(jī)磷類農(nóng)藥為分析對(duì)象,考察了吸附劑的用量和凈化時(shí)間,并將NPC與商業(yè)化材料N-丙基乙二胺(PSA)、十八烷基硅膠鍵合相(C18)和石墨化碳黑(GCB)進(jìn)行了對(duì)比。結(jié)果表明,NPC最佳使用量為0.01 g,凈化時(shí)間只需2 min。NPC成本遠(yuǎn)低于C18、PSA和GCB,因具有豐富的孔道結(jié)構(gòu),NPC凈化效果顯著優(yōu)于3種商業(yè)化材料。在最優(yōu)條件下,14種有機(jī)磷農(nóng)藥在0.02~1.0 mg/L范圍內(nèi)的線性關(guān)系良好(R20.99),檢出限(S/N=3)為0.63~5.30μg/kg。3個(gè)添加水平下的平均回收率為71.3%~114.7%,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為0.9%~12.9%。本方法操作簡(jiǎn)便、快速、成本低,在果蔬樣品前處理中具有廣闊的應(yīng)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.
【作者單位】： 西南大學(xué)園藝園林學(xué)院;南方山地園藝學(xué)教育部重點(diǎn)實(shí)驗(yàn)室;重慶出入境檢驗(yàn)檢疫局;
【基金】：重慶市現(xiàn)代農(nóng)業(yè)特色產(chǎn)業(yè)技術(shù)體系:晚熟柑橘產(chǎn)業(yè)技術(shù)體系(No.20174-4) 2016食用農(nóng)產(chǎn)品特征性營(yíng)養(yǎng)組成識(shí)別與驗(yàn)證評(píng)估專項(xiàng)(No.GJFP201601501,No.GJFP201601503)資助
【分類號(hào)】：O657.71;TS255.7

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