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目的研究应用反相高效液相色谱荧光检测器直接测定生活饮用水中氨基甲酸酯农药残留量的方法。方法采用Oasis HLB固相萃取柱富集浓缩生活饮用水中的氨基甲酸酯农药,柱温为40℃,以甲醇-水(55∶45,V/V)为流动相进行等度洗脱,流速为1.00 ml/min,以Symmetry C18柱(4.6 mm×250 mm,5μm)为分析柱,采用荧光检测器直接测定生活饮用水中氨基甲酸酯农药的含量,无需柱后衍生设备进行化学衍生化反应。结果当呋喃丹、甲萘威的浓度为0.050μg/ml~10.00μg/ml时,线性关系良好,相关系数(r)>0.999。检出限分别为0.16μg/L、0.07μg/L。在高、中、低3种浓度水平下,呋喃丹、甲萘威的平均加标回收率分别为89.4%~90.9%、90.5%~93.6%,相对标准偏差(RSD)分别为3.72%~8.50%、4.35%~7.14%。结论应用研究的新方法能够满足生活饮用水中氨基甲酸酯农药残留量的测定要求,方法简便、准确、快速、高效,易于在基层实验室实施。
Objective To study the method of direct determination of carbamate pesticide residues in domestic drinking water by reversed-phase high performance liquid chromatography with fluorescence detector. Methods Oasis HLB solid phase extraction (SPE) column was used to enrich carbamate pesticides in drinking water. The column temperature was 40 ℃ and the mobile phase was isocratic elution with methanol - water (55:45, V / V) The flow rate was 1.00 ml / min. A Symmetry C18 column (4.6 mm × 250 mm, 5 μm) was used as the analytical column. The fluorescence detector was used to directly determine the content of carbamate pesticides in domestic drinking water without chemical derivatization The reaction. Results When the concentrations of carbofuran and carbaryl were 0.050μg / ml ~ 10.00μg / ml, the linearity was good with the correlation coefficient (r)> 0.999. The detection limits were 0.16μg / L, 0.07μg / L respectively. The average recoveries of carbofuran and carbaryl were 89.4% -90.9% and 90.5% -93.6%, respectively, and the relative standard deviations (RSDs) were 3.72% ~ 8.50 at high, medium and low levels respectively %, 4.35% ~ 7.14%. Conclusion The new method of applied research can meet the requirement of determination of carbamate pesticide residues in drinking water. The method is simple, accurate, rapid, efficient and easy to implement in the laboratory.