GC Determination of 3 Organophosphorus Pesticides and Herbicide Atrazine in Soil with Accelerated Solvent Extraction
摘 要
提出了气相色谱法测定土壤中莠去津和3种有机磷农药敌敌畏、甲拌磷和乐果的含量的方法。样品经粉碎后用丙酮-二氯甲烷(1+1)混合溶剂经加速溶剂萃取仪在60 ℃静态萃取10 min。采用Rtx-1701色谱柱分离,火焰光度检测器测定3种有机磷农药;采用Rtx-CLP II色谱柱分离,电子捕获检测器测定莠去津。结果表明:加速溶剂萃取比超声提取法处理样品的回收率高。敌敌畏、甲拌磷、乐果和莠去津的检出限(3S/N)分别为0.08,0.07,0.09,0.40 μg·kg-1。以空白土壤样品为基体,进行加标回收试验,回收率在82.0%~106.0%之间,相对标准偏差(n=7)在10.5%~16.9%之间。
Abstract
The contents of atrazine and three organophosphorus pesticides, i.e., dichlorophos, phorate and dimethoate, in soil were determined by GC. The sample was crushed and extracted statically with mixed solvent of acetone+dichloromethane (1+1) at 60 ℃ for 10 min. The Rtx-1701 column and flame photometric detector were used for separation and determination of the 3 organophosphorus pesticides; and Rtx-CLP II column and electron capture detector were used for separation and determination of atrazine. It was found that recovery of accelerated solvent extraction was better than ultrasonic extraction. Detection limits (3S/N) of the method were found 0.08 μg·kg-1 for dichlorophos, 0.07 μg·kg-1 for phorate, 0.09 μg·kg-1 for dimethoate, 0.40 μg·kg-1 for atrazine. Using blank sample of soil as matrix, test for recovery was made by standard addition method, and values of recovery obtained were in the range of 82.0%-106.0%, with values of RSD′s (n=7) in the range of 10.5%-16.9%.
中图分类号 O657.7
所属栏目
基金项目 国土资源部地质大调查项目资助(1212010913004)
收稿日期 2010/12/21
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备注王娜(1980-),女,辽宁鞍山人,工程师,硕士研究生,从事有机分析测试工作。
引用该论文: WANG Na,LI Li-jun,WANG Yin-fu,WANG Hai-jiao. GC Determination of 3 Organophosphorus Pesticides and Herbicide Atrazine in Soil with Accelerated Solvent Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(2): 215~218
王娜,李丽君,汪寅夫,王海娇. 加速溶剂萃取-气相色谱法测定土壤中三种有机磷农药和除草剂莠去津[J]. 理化检验-化学分册, 2012, 48(2): 215~218
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【2】龚勇,秦冬梅.莠去津在土壤中的残留试验研究[J].农药科学与管理, 1999,20(4):35-37.
【3】任晋,蒋可,徐晓白.土壤中莠去津及其降解产物的提取及高效液相色谱-质谱分析[J].色谱, 2004,22(2):147-150.
【4】齐文启.环境监测新技术[M].北京:化学工业出版社, 2004.
【5】MAJORS R E. An overview of sample preparation methods for solids[J]. LC-GC, 1999,17(6):128-131.
【6】仲维科,郝戮,樊耀波,等.食品农药残留分析进展[J].分析化学, 2000,28(7):904-910.
【7】LPPEZ-AVILA V, BENEDICTO J, MLBAUER K. Stability of organochlorine and organophosphorus pesticides when extracted from solid matrixes with microwave energy[J]. J AOAC Int, 1998,81(6):1224-1232.
【8】万益群,陈宗保.土壤中多种有机磷及氨基甲酸酯类农药残留量的气相色谱-质谱法测定[J].分析科学学报, 2006,22(5):551-554.
【9】乔雄梧,马利平.土壤中残留的阿特拉津及其代谢产物的高效液相色谱和气-质谱联用分析[J].色谱, 1995,13(3):170-173.
【10】EPA SW-846Test methods for evaluating solid waste, method 3545[S].
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