作者：康彭¹, 朱霞萍¹, 张贵¹, 李军亚²

作者单位：1. 成都理工大学材料与化学化工学院，四川 成都 610059;
2. 四川省地质矿产勘查开发局四0五地质队，四川 成都 611830

关键词：Mg-Al-Fe-LDH;固相萃取;气相色谱质谱法;有机磷农药

摘要：

建立镁铝铁层状金属氢氧化物（Mg-Al-Fe-LDH）复合材料固相萃取气相色谱质谱法（GC-MS）测定水中的敌敌畏，乐果，氯吡硫磷，水胺硫磷的分析方法。复合材料用量为2 g，萃取12 min，二氯甲烷作为洗脱剂，洗脱剂用量为2 mL，洗脱时间1 min，4种农药的质量浓度在0.01~10 ng/mL范围内与峰面积线性关系良好，相关系数均大于0.99，方法相对标准偏差在1.1%~3.6%之间，检出限范围为0.001~0.03 ng/mL。测定稻田水中敌敌畏、乐果、氯吡硫磷和水胺硫磷的加标回收率在95.0%~120.0%之间，相对标准偏差在1.2%~6.5%之间。Mg-Al-Fe-LDH中铁取代部分铝进入层板，Fe³⁺的4s能级上有空轨道，可以与有机磷农药中含有孤对电子的磷和硫生成配位键，进一步增强对农药的吸附能力。基于Mg-Al-Fe-LDH固相萃取建立的分析方法检出限低，准确度高，能够满足水体中痕量有机磷农药的测定要求。

Study on solid phase extraction of organophosphorus pesticides with magnesium-aluminum-iron layered metal hydroxides
KANG Peng¹, ZHU Xiaping¹, ZHANG Gui¹, LI Junya²
1. College of Materials and Chemistry & Chemical Engineering, Chengdu University of Technology, Chengdu 610059, China;
2. 405 Geological Team, Sichuan Geological and Mineral Exploration and Development Bureau, Chengdu 611830, China
Abstract: A method for the determination of dichlorvos, dimethoate, chlorpyrifos and isocarbophos in water by solid phase extraction gas chromatography-mass spectrometry (GC-MS) with magnesium-aluminum-iron layered metal hydroxide (Mg-Al-Fe-LDH) composite was established. When the amount of Mg-Al-Fe-LDH was 2 g, the extraction time was 12 minutes, the eluant was 2 mL dichloromethane, and the elution time was 1 min, the mass concentration of four pesticides in the range of 0.01-10 ng/mL had a good linear relationship with the peak area, the correlation coefficients were greater than 0.99, and the relative standard deviation were 1.1%-3.6% and the detection limit of the method were 0.001-0.03 ng/mL. The recovery rate are 95.0%-120%, and the relative standard deviation  are 1.2%-6.5%. Iron replaces part of the aluminum into the laminate in Mg-Al-Fe-LDH. Fe³⁺ has empty orbits at the 4s energy level, which can form coordination bonds with phosphorus and sulfur containing lone pairs of electrons in organic phosphorus pesticides, further enhancing Adsorption capacity. The method based on Mg-Al-Fe-LDH solid phase extraction has low detection limit and high accuracy which can meet the determination requirements of trace organophosphorus pesticides in water.
Keywords: Mg-Al-Fe-LDH;solid phase extraction;GC-MS;organophosphorus pesticides
2021, 47(1):68-75  收稿日期: 2020-04-20;收到修改稿日期: 2020-06-04
基金项目: 四川省科技厅科技计划项目（2019YFN0148）
作者简介: 康彭(1993-),男,四川南充市人,硕士研究生,专业方向为分析化学
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