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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 被引量:11

HPLC multi-residue analysis of 13 N-methylcarbamates in traditional Chinese medicines with gel permeation chromatography and postcolumn derivatization
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摘要 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.
出处 《药物分析杂志》 CAS CSCD 北大核心 2010年第4期668-672,共5页 Chinese Journal of Pharmaceutical Analysis
关键词 凝胶渗透色谱 柱后衍生 荧光检测 N-甲基氨基甲酸酯农药 中药材 GPC postcolumn derivatization fluorescence detection N-methylcarbamate traditional Chinese medicine
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  • 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 pestieides 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 8321 B, Solvent- Extractable Nonvolatile Compounds By High -Performance Liquid Chromatography/Thermospray/Mass Spectrometry ( HPLC/ TS/MS) Or Ultraviolet(UV) Detetion.
  • 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).
  • 9梁祈,颜庆嫦.中药材黄芪中氨基甲酸酯农药残留量的毛细管气相色谱法测定[J].分析测试学报,1999,18(2):66-68. 被引量:31
  • 10董顺玲,胡家炽,何志强,杨仲元.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[J].药物分析杂志,2002,22(3):178-182. 被引量:34

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