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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 To establish a method for the determination of pesticide residues in dithiocarbamates (DTCs) in mushrooms. Methods L-cysteine hydrochloride and EDTA-Na2 mixture were used for the extraction and derivatization with 0.05 mol / L methyl iodide-chloroform-n-hexane solution. The derivatization, concentration, amino column purification, C18 column separation, Chromatography - UV detector detection. Results The linear range of the three kinds of DTCs pesticides was 0.25 mg / L ~ 5.0 mg / L and the correlation coefficient was 0.998. The detection limits and the minimum detectable concentrations were 0.02 mg / L and 0.015 mg / kg, respectively , 0.04 mg / L, 0.03 mg / kg, 0.08 mg / kg and 0.06 mg / kg for EBs, with the average recovery of 77% ~ 98% and the relative standard deviation of 2.2 % ~ 9.6%. Conclusion This method is effective and selective for the separation of three types of DTCs pesticide derivatives. The method is not easy to produce false positive results, and the results are accurate and reliable, which can meet the detection requirements of such pesticide residues (MRLs).