大豆氧化乐果残留分析方法的研究

STUDY ON ANALYSIS METHOD OF OMETHOATE RESIDUES IN SOYBEAN

采用HP1100型液相色谱仪,进行了大豆氧化乐果残留分析方法和分析条件的探讨,结果表明,以获取理想的分离度为目标,综合各项因素,最适宜的分析条件为:色谱柱为LUNA5μC18150mm×4.6mm;流动相为乙腈/水=6/94(V/V);检测波长为220nm;进样量为50μl;流速为1ml/min;柱温为室温(±25℃)。用甲醇-水和丙酮-水做提取液,用二氯甲烷做萃取剂从大豆及土壤中回收氧化乐果,并用液相色谱紫外检测器外标法定量测定其残留量,方法最小检出量低,迭0.108ng,最低检出浓度大豆植株和子粒可达2μg/kg,土壤可达0.4μg/kg。添加回收率为87.3%-101.5%;变异系数为0.99-16.98%。说明氧化乐果残留HPLC分析法是一个精度较高的新方法。

The method and conditions on analysing omethoate residues of soybean were studied with HPLC1100. The results showed that the superior analysis conditions were as follows: chromatographic pillar was LUNA5μC18 150mm×4. 6mm, fluid solution was a mixture of CH3CN/ water 6/94(V/V), measuring wavelength was 220nm} entering sample quantity was 50μl, flowing speed was 1ml/min, pillar temperature was±25℃. The method in this article was certificated to be applied with the minimum checking-out value of 0.108ng, the minimum concentration 2μg/kg in plants and seeds of soybeans as well as 0. 4μg/kg in soil. The data by this method also showed that the recovery rate ranged from 87. 3% to 101. 5% and values of the CV were from 0. 99 % to 16. 98%. which conformed that analysing omethoate residues of soybeans by HPLC was a new way with high precision.