高效液相色谱法测定蔬菜中6种氨基甲酸酯类农药残留及降解规律的研究

Determination of 6 kinds of carbamate pesticide residues in vegetables by high performance liquid chromatography and research on degradation rule

中文关键词:  高效液相色谱法  氨基甲酸酯  农药

英文关键词:high performance liquid chromatography  vegetables  carbamate  pesticide  degradation rule

中文摘要:

      目的 建立高效液相色谱法(high performance liquid chromatography, HPLC)测定蔬菜中6种氨基甲酸酯类农药残留量的分析方法, 并研究氨基甲酸酯类农药在蔬菜中的降解规律。方法 样品经乙腈打浆提取氨基甲酸酯类农药, 上清液经固相吸附剂净化, 浓缩干后用甲醇定容, 采用HPLC-柱后衍生法进行定量分析。结果 方法经优化发现6种氨基甲酸酯类农药在0.10~2.00 μg/mL质量浓度范围内峰面积与浓度呈良好线性关系, 相关系数均不小于0.9996, 检出限为0.002~0.005 mg/kg, 平均回收率为86%~95%, 相对标准偏差均小于3.5%。同时得到氨基甲酸酯类在蔬菜中的残留状况与降解规律, 发现灭多威农药残留含量的大小顺序为: 无清洗过的土豆皮>清洗过的土豆皮>土豆内部。结论 本方法灵敏度高、检出限低、回收率好、操作可行, 满足实验要求。农药残留降解规律具有显著差异性, 为评价氨基甲酸酯类农药使用后的蔬菜的安全性提供理论依据。

英文摘要:

      Objective To establish a method for the determination of 6 kinds of carbamate pesticide residues in vegetables by high performance liquid chromatography (HPLC), and study the degradation rule of carbamate pesticides in vegetables. Methods The samples were extracted with acetonitrile to extract carbamate pesticides. The supernatant was purified by solid phase adsorbent, concentrated and dried, and then diluted with methanol. The quantitative analysis was carried out by HPLC-post column derivatization. Results Through optimization of the method, it was found that there was a good linear relationship between peak area and concentration of 6 kinds of carbamate pesticides in the mass concentration range of 0.10–2.00 μg/mL, with correlation coefficients not less than 0.9996. The limit of detection was 0.002–0.005 mg/kg, the average recovery rate was 86%–95%, and the relative standard deviation was less than 3.5%. At the same time, the residual status and degradation rule of amino esters in vegetables were obtained, and it was found that the order of pesticide residue content of methomyl was: Unwashed potato peel>washed potato peel>potato interior. Conclusion This method has high sensitivity, low limit of detection, good recovery rate and feasible operation, meeting the experimental requirements. The degradation rules of pesticide residues show significant differences, providing a theoretical basis for evaluating the safety of vegetables after the use of carbamate pesticides.