[1]刘腾飞,张丽,杨代凤,等.茶园土壤中拟除虫菊酯类农药残留检测[J].江苏农业学报,2015,(04):935-941.[doi:10.3969/j.issn.1000-4440.2015.04.036]
　LIU Teng-fei,ZHANG Li,YANG Dai-feng,et al.Determination of pyrethroid pesticides residues in tea-planted soil[J].,2015,(04):935-941.[doi:10.3969/j.issn.1000-4440.2015.04.036]
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茶园土壤中拟除虫菊酯类农药残留检测()
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江苏农业学报[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2015年04期
页码:
935-941
栏目:
加工贮藏·质量安全
出版日期:
2015-08-31

文章信息/Info

Title:
Determination of pyrethroid pesticides residues in tea-planted soil
作者:
刘腾飞1; 张丽2; 杨代凤1; 董明辉1; 顾俊荣1
（1.江苏太湖地区农业科学研究所,江苏苏州215155;2.苏州市职业大学,江苏苏州215104）
Author(s):
LIU Teng-fei1; ZHANG Li2; YANG Dai-feng1; DONG Ming-hui1; GU Jun-rong1
(1.Institute of Agricultural Sciences of Lake Taihu Area in Jiangsu Province, Suzhou 215155, China;2.Suzhou Vocational University, Suzhou 215104, China)
关键词:
茶园土壤; 拟除虫菊酯农药; 残留; 分散固相萃取; 气相色谱-电子捕获法
Keywords:
tea-planted soil; pyrethroid pesticide; residue; despersive solid phase extraction(DSPE); gas chromatograph-electron captured detection(GC-ECD)
分类号:
X592. 02
DOI:
10.3969/j.issn.1000-4440.2015.04.036
文献标志码:
A
摘要:
采用乙酸-乙腈溶液（体积比1∶99）超声提取，乙二胺-N-丙基硅烷和十八烷基硅烷键合硅胶吸附剂进行分散固相萃取净化，建立了气相色谱-电子捕获法（GC-ECD），用该方法检测了土壤中甲氰菊酯、高效氯氟氰菊酯、氯菊酯、氟氯氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯7种拟除虫菊酯类农药残留。结果显示，7种拟除虫菊酯类农药在 0.004～2.000 mg/L 范围内农药浓度与峰面积线性关系良好；7种农药在 0.01～0.50 mg/kg添加水平下，平均回收率为 91.6%～100.3%，相对标准偏差为 1.3%～9.8%，检出限为 0.001 8～0.008 8 mg/kg，定量限为 0.029 0～0.005 8 mg/kg。将该方法应用于16份茶园土壤样品中7种拟除虫菊酯类农药的残留测定，其中4份样品含有高效氯氟氰菊酯，含量为 0.007 5～0.013 4 mg/kg，1份样品含有氟氯氰菊酯，含量为0.038 mg/kg。该方法操作简单、结果准确、溶剂用量少、分析成本低，可以满足土壤中拟除虫菊酯类农药的检测需要。
Abstract:
A gas chromatograph-electron captured detection(GC-ECD) method was developed for simultaneous determination of fenpropathrin, lambda-cyhalothrin, permethrin, cyfluthrin, cypermethrin, fenvalerate and deltamethrin in soil based on the ultrasound assisted extraction of the sample with acetic acid-acetonitrile solution (volume ratio,1∶99 ) as solvent and the following purification by dispersive solid phase extraction (DSPE) using PSA (primary secondary amine) and C18 (octadecylsilane bonded silica) as adsorbents. Good linearities between concentrations and peak areas were achieved in the concentration range of 0.004-2.000 mg/L for target pesticides, with correlation coefficients higher than 0.999. The average recoveries of target pesticides in soil were 91.6%-100.3% with the relative standard deviations ranging from 1.3% to 9.8% in the spiked level of 0.01-0.50 mg/kg. The limits of detection (LOD) by means of matrix-matched external standard method for target pyrethroid pesticides were 0.001 8-0.008 8 mg/kg and the limits of quantification (LOQ) were 0.029 0-0.005 8 mg/kg. The method was employed to detect the 7 pyrethroid pesticides residues in the soil collected from local tea garden in Suzhou. Among 16 soil samples, lambda-cyhalothrin was detected in 4 samples with the content varying from 0.007 5 to 0.013 4 mg/kg, and cyfluthrin was detected in one sample with the content of 0.038 mg/kg. This method is simple, accurate, solvent saving and cost saving, and provides an easy way to simultaneously determine the pyrethroid pesticides in soil.

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备注/Memo

备注/Memo:
收稿日期：2015-01-22 基金项目：江苏省农业科技自主创新基金项目[SCX(14)2163] 作者简介：刘腾飞（1985-），男，江苏淮阴人，硕士，助理研究员,主要从事农产品农药残留检测技术研究工作。(Tel)0512-65388897;(E-mail) bbliutengfei@163.com 通讯作者：杨代凤，（Tel）0512-66705835；（E-mail）szyangdf@163.com
更新日期/Last Update: 2015-08-31