分散固相萃取-气相色谱-质谱法测定农产品及产地土壤中均三氮苯类除草剂残留量
GC-MS Determination of Residual Amounts of S-Triazine Herbicides in Agricultural Products and Soil of Their Producing Area with Dispersive Solid Phase Extraction
摘 要
以冰乙酸-正己烷饱和乙腈溶液作萃取剂,以乙二胺-N-丙基硅烷(PSA)、C18、石墨化炭黑(Carb)为吸附剂对农产品及产地土壤中13种均三氮苯类除草剂进行分散固相萃取。提取液供气相色谱-质谱仪测定。在选择离子监测模式下,13种均三氮苯类除草剂的线性范围均为0.05~5 mg·L-1。西玛津和氰草津的测定下限(10S/N)为0.01 mg·kg-1,其余11种除草剂的测定下限为0.005 mg·kg-1。在0.01,0.1 mg·kg-1两个添加水平下进行回收试验,13种均三氮苯类除草剂的回收率在75.0%~111.8%之间,测定值的相对标准偏差(n=6)在3.2%~9.2%之间。
气相色谱-质谱法
均三氮苯类除草剂
农产品及产地土壤
Dispersive solid phase extraction
GC-MS
S-Triazine herbicides
Agricultural products and soil of their producing area
Abstract
Residual amounts of S-triazine herbicides in samples of agricultural products and the soil of their producing area were extracted by dispersive solid phase extraction (DSPE) with acetonitrile (saturated with glacial acetic acid and n-hexane) as extraction solvent and PSA, C18, Carb as adsorbent. The eluate was determined by GC-MS. Under the selection ion monitoring mode, linearity ranges for 13 S-triazine herbicides were between 0.05-5.0 mg·L-1, with lower limits of determination (10S/N) of 0.01 mg·kg-1 for simazine and cyanazine, and 0.005 mg·kg-1 for the others. Tests for recovery and precision were made by addition of 0.01 mg·kg-1 and 0.1 mg·kg-1 of standard solutions, and analyzed by the proposed method, values of recovery in the range of 75.0%-111.8% and values of RSD′s (n=6) in the range of 3.2%-9.2% were obtained.
中图分类号 O657.6
所属栏目 工作简报
基金项目 江苏出入境检验检疫局科研计划(2009KJ33)
收稿日期 2011/6/11
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联系人作者曹军(cj925928@126.com)
备注曹军(1982-),男,安徽怀宁人,工程师,主要从事食品检验检疫。
引用该论文: CAO Jun,YU Bo-hua,CHEN Yong,YANG Rui-zhang,WANG Tai-quan,ZENG Zheng-hong,ZHANG Dan,GAO Ling. GC-MS Determination of Residual Amounts of S-Triazine Herbicides in Agricultural Products and Soil of Their Producing Area with Dispersive Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(8): 959～961
曹军,于伯华,陈勇,杨瑞章,王太全,曾正宏,张丹,高玲. 分散固相萃取-气相色谱-质谱法测定农产品及产地土壤中均三氮苯类除草剂残留量[J]. 理化检验－化学分册, 2012, 48(8): 959～961
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