柱前衍生-HPLC法测定香菇中二硫代氨基甲酸盐类农药残留量  

Determination of dithiocarbamates residues in lentinus edodes by pre-column derivation HPLC

作　　者：贺东霞[1] 

机构地区：[1]南阳医学高等专科学校,河南南阳473058

出　　处：《中国卫生检验杂志》2014年第23期3354-3357,共4页Chinese Journal of Health Laboratory Technology

基　　金：河南省教育厅2011年度自然科学研究计划项目(20-11C330001)

摘　　要：目的建立香菇中二硫代氨基甲酸盐类(DTCs)农药残留量的测定方法。方法采用L-半胱氨酸盐酸盐和EDTA-Na2混合液进行提出,0.05 mol/L碘甲烷-氯仿-正己烷溶液萃取、衍生、浓缩,氨基小柱净化,C18柱分离,高效液相色谱-紫外检测器检测。结果 3类DTCs农药线性范围为0.25 mg/L^5.0 mg/L,相关系数r>0.998,方法检出限和最低检出浓度分别为:福美类(DMDs)0.02 mg/L、0.015 mg/kg,代森类(EBDs)0.04 mg/L、0.03 mg/kg,丙森类(PBDs)0.08 mg/L、0.06 mg/kg,平均加标回收率为77%~98%,相对标准偏差为2.2%~9.6%。结论本方法对3类DTCs农药衍生物分离效果好,选择性强,不易产生假阳性,测定结果准确可靠,能满足对该类农药残留限量(MRLs)的检测要求。Objective The research aimed to establish the method of measuring the quantity of dithiocarbamates（ DTCs） pesticide residue in lentinus edodes. Methods The complex samples were extracted by the mixed solution of L-cysteine and EDTA-Na2. Then 0. 05 mol / L methyl iodide in methenyl chloride-hexane was added into the extracts and the mixture was extracted,derived and concentrated. Carb-NH2clean-up,then the derivatives were separated on a Sunfire C18 column,tested by HPLC-UVD. Results The range of 3 kinds of dithiocarbamates（ DTCs） is（ 0. 25 - 5. 0） mg / L,the correlation coefficient r 〉0. 998, and the method detection limits and the minimum concentrations are： dimethyldithiocarbamates（ DMDs）,0. 02 mg / L,0. 015 mg / kg. ethylenebisdithiocarbamates（ EBDCs）,0. 04 mg / L,0. 03 mg / kg,Propylenebisdithiocarbamates（ PBDs） 0. 08 mg/L,0. 06 mg/kg,and the average recovery rate was 77% - 98%,and the relative standard deviation is 2. 2%- 9. 6%. Conclusion This method of separating the 3 kinds of DTCs pesticide derivatives has a better effect. It is more selective,and it is less likely to produce false positives. So the analysis result is accurate and reliable,which can meet the need of testing requirements on the pesticide residue of MRLs.

关 键 词：高效液相色谱 二硫代氨基甲酸盐类农药 测定 

分 类 号：O657.72[理学—分析化学]