凝胶渗透色谱-柱后衍生高效液相色谱法测定中药材中13种N-甲基氨基甲酸酯农药残留___

 

目的：建立了中药材中13种N-甲基氨基甲酸酯农药残留量的高效液相分析方法。方法：样品用丙酮提取，经凝胶渗透色谱净化，通过柱后衍生，荧光检测器测定农药残留量。结果：除涕灭威和涕灭威亚砜外，3个水平回收率均在75.7%~102.3%，相对标准偏差为0.4%~7.0%。方法检测限为0.01 mg·kg^-1，定量限为0.03 mg·kg^-1。在7种中药材中均未检出农药残留。结论：本方法灵敏，准确，适用于中药材中13种N-甲基氨基甲酸酯农药残留的检测。

 

Objective:To establish a method for determination of 13 N-methylcarbamates in traditional Chinese medicines.Method:The samples were extracted with acetone and cleaning up with GPC.The pesticides were separaed by HPLC with postcolumn derivatization and detected with fluorescence detector.Result:Except for aldicarb sulfoxide and aldicarb,the average recoveries in three levels were 75.7%-102.3% with relative standard deviations(RSD) between 0.4%-7.0%.The limits of detection(LOD) were 0.01 mg·kg^-1,and the limits of quantitation(LOQ) were 0.03 mg·kg^-1.The pesticide residues were not detected in all 7 kinds of TCMs.Conclusion:The method is sensitive,accurate and suitable for determination of 13 N-methylcarbamates residues in TCMs.

1AOAC Official Method 975.40,N-Methylcarbamate Insecticide Residues Gas Chromatographic Method.

2GB/T 5009.104-2003,Determination of carbamate pesticide residues in vegetable foods(植物性食品中氨基甲酸酯类农药残留量测定).

3GB/T 20796-2006,Method for determination of 405 pesticides and related chemicals residues in fruits and vegetables-LC-MS-MS method(水果和蔬菜中405种农药相关化学品残留量的测定-液相色谱-串联质谱法).

4United States Environmental Protection Agency Method 8321B,Solvent-Extractable Nonvolatile Compounds By High-Performance Liquid Chromatography/Thermospray/Mass Spectrometry(HPLC/TS/MS) Or Ultraviolet(UV) Detction.

5United States Environmental Protection Agency Method 531.2,Measurement Of N-Methylcarbamoyloximes And N-Methylcarbamates In Water By Direct Aqueous Injection HPLC with Postcolumn Derivatization.

6United States Environmental Protection Agency Method 8318A,N-Methylcarbamates By High Performance Liquid Chromatography(HPLC).

7AOAC Official Method 985.23,N-Methylcarbamate Insecticide and Metabolite Residues Liquid Chromatographic Method.

8NY/T 761-2008,Pesticide multiresidue screen methods for determination of organophosphorus pesticides,organochlorine pesticides,pyrethroid pesticides and carbamate pesticides in vegetables and fruits(蔬菜和水果中拟除去菊酯和氨基甲酸酯类农药的残留测定法).

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10DONG Shun-ling（董顺玲）,HH Jia-chi（胡家炽）,HE zhi-qiang（何志强）,et al.RP-HPLC determination of residual amount of aldicarb,carbofuran and carbaryl in Chiness crude drugs（中药材中氨基甲酸酯类农药残留量的反相高效液相色谱法）.Chin J Pharm Anal（药物分析杂志）,2002,22(3):178

11LIU Hong-cheng（刘宏程）,YANG Guang-yu（杨光宇）,MA Xue-tao（马雪涛）,et al.HPLC determination of residual carbamate insecticides in Chinese crude durgs post column derivation method（测定中药材中氨基甲酸酯类杀虫剂残留的高效液相色谱柱后衍生法）.Chin J Pharm Anal(药物分析杂志),2006,26(6):857