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目的建立固相萃取/高效液相色谱法测定生活饮用水中10种氨基甲酸酯类农药残留的分析方法。方法样品中氨基甲酸酯类农药用C18固相萃取小柱富集,净化,乙酸乙酯洗脱,氮气吹干甲醇定容,以甲醇+乙腈+水为流动相,经C18柱分离,0.05 mol/L氢氧化钠溶液水解,OPA溶液化学柱后衍生后,在激发波长为339 nm,发射波长为445 nm条件下,荧光检测器检测。结果各组分在0.02μg/ml~10μg/ml时,浓度与峰面积呈良好的线性关系,相关系数为0.9991~0.9997,方法检出限在0.08μg/L~0.12μg/L之间。在添加0.5μg/L~5μg/L的水平内,加标回收率在86.2%~100.4%之间,相对标准偏差在2.1%~9.3%之间。结论该方法准确度高、精密度好,灵敏度高、检出限低,线性范围宽,干扰少,可用于生活饮用水及其水源水中氨基甲酸酯类农药检测。
OBJECTIVE To establish a method for the determination of 10 carbamate pesticides in domestic drinking water by solid phase extraction and high performance liquid chromatography. Methods Carbamates were enriched in C18 solid phase extraction cartridges, purified and eluted with ethyl acetate. The methanol was denatured by nitrogen and methanol was extracted with methanol, acetonitrile and water. The residue was separated on a C18 column and eluted with 0.05 mol / L sodium hydroxide solution hydrolysis, OPA solution chemical column after derivatization, the excitation wavelength of 339 nm, the emission wavelength of 445 nm conditions, the fluorescence detector detection. Results The results showed that there was a good linear relationship between the concentration and the peak area in the range of 0.02μg / ml ~ 10μg / ml, the correlation coefficient was 0.9991 ~ 0.9997, the detection limit was 0.08μg / L ~ 0.12μg / L. The spiked recoveries ranged from 86.2% to 100.4% and the relative standard deviations (RSDs) ranged from 2.1% to 9.3% with the addition of 0.5μg / L ~ 5μg / L. Conclusion The method has high accuracy, good precision, high sensitivity, low detection limit, wide linear range and less interference. It can be used for the detection of carbamate pesticides in domestic drinking water and its source water.