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
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.
Keywords：phenoxy carboxylic acid; gas chromatography-mass spectrometry; extract; derivatizationr
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.