建立了中草药中有机磷和氨基甲酸酯类农药残留量同时检测的气相色谱分析方法。中药材试样依据正交实验的优化条件,用V(C6H14):V(丙酮)=1:1混合提取剂进行超声波提取,经弗罗里硅土和中性氧化铝层析柱净化后,采用HP.5毛细管柱分离,氮磷检测器同时检测中草药中15种有机磷和7种氨基甲酸酯类农药残留量。22种农药在0.015~1.0mg/L范围内线性良好,线性相关系数为0.9950—1.000,在0.05、0.1mg/kg两个添加水平的平均回收率分别为70.6%。128.6%和69.5%。116.1%,相对标准偏差分别为0.98%。18%和0.37%~15%。各种农药的检出限为0.002~0.015mg/L。方法已用于中草药中有机磷和氨基甲酸酯类农药残留量的同时检测。
A simple and quick method for the detennination of 15 organophosphorus and 7 carbamate pesticide residues in chinese herbal medicine by GC-NPD has been proposed. Extraction conditions were optimized using orthogonal experimental design. The 22 pesticide residues in chinese herbal medicine were extracted by ultrasonic with hexane-acetone ( 1 : 1, V/V). Extracted liquid was cleaned up by a column filled with florisil and neutral aluminum oxide. And the analytical screening was determined by gas chromatography using HP-5 capillary column equipped with a nitrogenphosphorus detector. The results presented the excellent linearity between analytical signal and analyte concentration in the range of 0.015- 1.0 mg/L, and the linear correlation coefficients were 0.9950 - 1.000. The average recoveries obtained from samples spiked with standards at the concentration levels of 0.05 and 0.1 mg/kg were in the range of 70.6%- 128.6% and 69.5% - 116.1%, respectively, with relative standard deviations of 0.98% ~ 18% and 0.37% - 15%, respectively. Limits of detection were 0.002 - 0.015 mg/L. A satisfactory result was obtained in the simultaneous determination of organophesphorus and carbamate pesticide residues in chinese herbal medicine.