溶液吸收-气相色谱质谱测定天麻中二硫代氨基甲酸酯(盐)类农药的含量

目的 建立溶液吸收-气相色谱质谱检测法测定天麻中二硫代氨基甲酸酯(盐)类农药残留量的方法。方法 目标物在加热条件下经溶液吸收, 转化为二硫化碳, 经正己烷萃取, 采用气相色谱质谱法间接测定二硫代氨基甲酸酯(盐)类农药含量。对云南省16州市采集的55件天麻中的二硫代氨基甲酸酯(盐)类农药的残留量进行统计分析。结果 该方法的线性范围为0.02~10 mg/kg, 相关系数0.9996, 定量限0.010 mg/kg, 空白基质加标回收率90.5%~105.0%, 相对标准偏差(relative standard deviation, RSD)为4.77% (n=6)。55件天麻样品检出率23.6%, 平均值0.021 mg/kg, 含量范围为ND~0.275 mg/kg。结论 该方法简便、快速、灵敏, 适合天麻中二硫代氨基甲酸酯(盐)类农药的测定。采集的天麻样品中二硫代氨基甲酸酯(盐)类农残含量水平总体较低。

Determination of dithiocarbamate (salt) pesticides in Gastrodiaelata by solution absorption-gas chromatography-mass spectrometry

Objective To establish a method of determination of dithiocarbamate (salt) pesticides in Gastrodiaelata by solution absorption-gas chromatography-mass spectrometry. Methods The target substance was absorbed by the solution under heating, converted into carbon disulfide, extracted by n-hexane, and the content of the dithiocarbamate (salt) pesticide was indirectly determined by gas chromatography-mass spectrometry. The residual amount of dithiocarbamate (salt) pesticides in 55 gastrodia collected in 16 cities of Yunnan province was statistically analyzed. Results The linear range of the method was 0.02?10 mg/kg, the correlation coefficient was 0.9996, the limit of quantification was 0.010 mg/kg, the recovery rate of blank matrix was 90.5%?105.0%, and the relative standard deviation (RSD) was 4.77% (n=6). The detection rate of 55 gastrodia samples was 23.6%, the average value was 0.021 mg/kg, and the content range was ND~0.275 mg/kg. Conclusion This method is simple, rapid and sensitive, which is suitable for the determination of dithiocarbamate (salt) pesticides in Gastrodiaelata. The level of dithiocarbamate (residue) pesticide residues in the collected Gastrodiaelata samples was generally low.