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    高效液相色谱法测定农药产品中非法添加的限制性农药氨基甲酸酯的含量

    Determination of Restricted Pesticides-Carbamates Illegally Added in Pesticide Products by High Performance Liquid Chromatography

    • 摘要: 农药样品0.400 g于甲醇80 mL中超声溶解10 min。用甲醇定容其体积为100.0 mL,分取部分溶液(约50 mL),离心分离5 min,取其上清液过0.45 μm滤膜过滤,滤液供高效液相色谱法分析。选用Besil C18-B色谱柱为固定相,柱温为30℃,以不同比例的(A)水和(B)甲醇组成的混合液为流动相,以1 mL·min-1的流量进行梯度洗脱,使样品中添加的12种限制使用的氨基甲酸酯类农药完全分离;采用二极管阵列检测器,在波长215 nm处检测。结果表明:12种氨基甲酸酯农药的浓度在5.0~100.0 mg·L-1内与其峰面积呈线性关系,检出限(3S/N)在0.1~0.2 mg·kg-1之间。以空白农药样品为基质,按标准加入法进行回收试验,回收率在97.2%~106%之间,测定值的相对标准偏差(n=6)在1.5%~3.8%之间。

       

      Abstract: Pesticide sample (0.400 g) was dissolved ultrasonically in 80 mL of methanol for 10 min, and the solution was diluted to 100.0 mL with methanol. An aliquot of the sample solution (ca. 50 mL) was taken and centrifuged for 5 min. The supernatant was taken and filtered through a filtering membrane of 0.45 μm. The filtrate was used for HPLC analysis. Besil C18-B column was selected as stationary phase with column temperature at 30℃. Mixtures of (A) water and (B) methanol in various proportions were used as mobile phase in gradient elution with a flow rate of 1 mL·min-1, to effect a satisfactory separation of the 12 carbamates. UV-detection was made at the wavelength of 215 nm using diode array detector. As shown by the results, linear relationships between values of peak area and mass concentration of the 12 carbamate pesticides in the range of 5.0-100.0 mg·L-1, with detection limits (3S/N) in the range of 0.1-0.2 mg·kg-1. Test for recovery by standard addition method was made using a blank pesticide sample as matrix, giving results in the range of 97.2%-106%, and RSDs (n=6) ranged from 1.5% to 3.8%.

       

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