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建立了硫丹(Endosulfan)在苹果中残留分析方法。样品用30 ml丙酮:乙酸乙酯(9:1)提取,5 g 5%水脱活处理的Florisi L(含活性炭)柱层析净化,气相色谱测定。硫丹3种单体的最小检测量分别为10~(-11)、10~(-11)、2.5×10~(-11)g。苹果样品中α-硫丹的添加回收率为86.54%~95.34%,变异系数为1.45%~4.73%;β-硫丹的添加回收率为82.91%~100.63%,变异系数为1.39%~4.72%;硫丹硫酸酯82.22%~101.15%,变异系数为0.75%~3.99%。方法的最低检出浓度分别为2.5×10~(-3)mg/kg,2.5×10~(-3)mg/kg,6.25×10~(-3)mg/kg。该方法的准确度、精确度、灵敏度均达到农药残留分析的要求。
Endosulfan was established in apple residue analysis. Samples were extracted with 30 ml of acetone: ethyl acetate (9: 1) and purified on a Florisi L column containing 5 g of 5% deactivated water by gas chromatography. The minimum detectable levels of endosulfan were 10 ~ (-11), 10 ~ (-11), 2.5 × 10 ~ (-11) g, respectively. The recoveries of α-endosulfan in apple samples ranged from 86.54% to 95.34% and the coefficients of variation ranged from 1.45% to 4.73%. The recoveries of β-endosulfan were 82.91% -100.63% and the coefficients of variation were 1.39% -4.72% ; Endosulfan sulfate 82.22% ~ 101.15%, coefficient of variation of 0.75% ~ 3.99%. The minimum detectable concentration was 2.5 × 10 ~ (-3) mg / kg, 2.5 × 10 ~ (-3) mg / kg and 6.25 × 10 ~ (-3) mg / kg, respectively. The accuracy, precision and sensitivity of this method all meet the requirements of pesticide residue analysis.