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《化学分析计量》 2017年第04期
DOI:10.3969/j.issn.1008-6145.2017.04.003
气相色谱-质谱法测定棉花中苯氧羧酸类除草剂
徐东峰1,刘伯韬2,卢晓东1
1. 山东省纤维检验局; 2. 山东大学公共卫生学院 
Determination of Phenoxy Carboxylic Acid Herbicides in Cotton by GC-MS
Xu Dongfeng1,Liu Botao2,Lu Xiaodong1
1. Shandong Bureau of Fiber Inspection, Jinan 250021, China; 2. School of Public Health, Shandong University, Jinan 250012, China 
摘要: 采用气相色谱-质谱联用法检测棉花中3种苯氧羧酸类除草剂[2,4-D,  2,4,5-T,  2-甲-4-氯丁酸(MCPB)]的残留量。样品用甲酸酸化的丙酮提取,硫酸催化甲酯化反应,用气相色谱-质谱联用仪测定。采用HPLC法与GC-MS法对提取与衍生化步骤进行优化。2,4-D,  2,4,5-T,  MCPB 3种化合物在0.075~7.5 mg/kg范围内线性均良好,检出限分别为0.5,0.5,0.8 μg/kg,测定结果的相对标准偏差分别为4.1%,4.3%,4.0%(n=5),方法回收率分别为93.6%,95.5%,93.9%。该方法各项指标均可满足检测要求。  
Abstract:A method for detection of 2, 4-D, 2, 4, 5-T, 2-a,-4-butyric acid (MCPB) residue in cotton was established. The samples were extracted by acetone acidized by formic acid, methyl esterification was catalyzed by sulfuric acid, then determined with gas chromatography-mass spectrometry. The extraction and derivatization steps were optimized by HPLC and GC-MS. The results showed that fine linearity was found in the range of 0.075-7.5 mg/kg for 2, 4-D; 2, 4, 5-T and MCPB, the detection limits were 0.5, 0.5, 0.8μg/kg, repectively. The relative standard deviations of detection results of 2, 4-D; 2, 4, 5-T, MCPB were 4.1%, 4.3%, 4.0%(n=5), and the recoveries were 93.6%, 95.5%, 93.9%, respectively. All indexes of this method can meet the requirement of test. 
关键词:苯氧羧酸;气相色谱-质谱法;提取;衍生化 
Keywords:phenoxy carboxylic acid; gas chromatography-mass spectrometry; extract; derivatizationr 
基金:山东省质量技术监督局科研项目(2016KY17) 
本文引用格式:
徐东峰,刘伯韬,卢晓东.气相色谱-质谱法测定棉花中苯氧羧酸类除草剂[J].化学分析计量,2017,26(4):13-16.
XU D F,LIU B T,LU X D .Determination of Phenoxy Carboxylic Acid Herbicides in Cotton by GC-MS[J]. Chemical analysis and meterage,2017,26(4):13-16. 

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