作者：杨敬坡1,2, 王文军3, 郭延凯1,2, 陈晓轩1,2, 都泽铭1,2
作者单位：1. 河北科技大学环境科学与工程学院, 河北 石家庄 050018;
2. 河北省污染防治生物技术实验室, 河北 石家庄 050018;
3. 保定学院汽车与电子工程学院, 河北 保定 071051
关键词：QuEChERS;苹果;土壤;菊酯
摘要：
实验建立利用QuEChERS提取苹果种植土壤中的5种菊酯类农药（甲氰菊酯、联苯菊酯、高效氯氟氰菊酯、氯菊酯、氰戊菊酯），气相色谱-质谱法定性定量检测的分析方法。苹果种植土壤样品用乙腈：冰乙酸（9：1，V/V）进行超声提取，QuEChERS方法进行净化处理，净化后的溶液用氮吹仪吹干，残渣用丙酮溶解定容至1 mL，0.45 m滤膜过滤，GC-MS仪定性定量检测。结果表明：5种菊酯类农药在0.1~50.0 g/mL范围内线性关系良好，r2均大于0.995；检出限在0.008~0.02 mg/kg之间，加标回收率范围为80.6%~106.7%；精密度相对标准偏差在1.8%~2.8%之间，重复性相对标准偏差在3.5%~4.6%之间。实验证明该方法具有前处理简单、检测速度快、灵敏度高、检测结果准确等优点。
QuEChERS-GC/MS method for determination of 5 pyrethroid pesticide residues in planting soil of apple
YANG Jingpo1,2, WANG Wenjun3, GUO Yankai1,2, CHEN Xiaoxuan1,2, DU Zeming1,2
1. School of Environmental Science and Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, China;
2. Pollution Prevention Biotechnology Laboratory of Hebei Province, Shijiazhuang 050018, China;
3. College of Automobile and Electronic Engineering, Baoding College, Baoding 071051, China
Abstract: A QuEChERS pr-treatment method for extracting 5 pyrethroid pesticide residues (fenpropathrin, bifenthrin, lambda-cyhalothrin, permethrin and fenvalerate) in planting soil of apple and GC/MS method for determination quantitatively was established. Planting soil of apple samples were ultrasoned and extracted by acetonitrile:glacial acetic acid (9:1,V/V), QuEChERS was used for sample purifying. Purification solution was firstly concentrated to dry under nitrogen, then the residue was dilute with acetone to 1 mL, filtered with 0.45 μm filter membrane and detected qualitatively and quantitatively by GC/MS. It was showed that concentration of 5 pyrethroid pesticide showed good linear relationships in the range 0.1-50.0 μg/mL, the correlation coefficients were all above 0.995. The detection limits were bewteen 0.008-0.02 mg/kg and the recoveries were ranged from 80.6%-106.7%. RSD of precision were ranged from 1.8%-2.8%, Repeatability of the relative standard deviation (RSD) of 6 pesticide residues were 3.5%-4.6%. This method was proved to be simple and quick pre-treated with high sensitivity and accuracy.
Keywords: QuEChERS;apple;soil;pyrethroid
2018, 44(11): 71-76 收稿日期: 2018-08-21;收到修改稿日期: 2018-09-28
基金项目: 河北省科技支撑计划项目（15273610D）；河北省社会科学发展研究课题民生调研专项（201701410）；河北科技大学16PT基金（2016PT43）
作者简介: 杨敬坡(1978-),男,河北保定市人,高级实验师,硕士,研究方向为土壤修复
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