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lvshidong

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[求助] 农药残留前处理和计算求助,谢谢大家

大家好,最近在用GC-MS-SIM做糙米中的农药残留,主要是敌敌畏、甲拌磷、马拉硫磷、毒死蜱、三唑磷和氯氢菊酯。现在把前处理方法说一下,麻烦大家帮我看看对不对,十分感谢。

准确称取20g试样,加入50.0mL乙腈,振荡30min后用滤纸过滤,滤液收集到装有5-7gNacl的锥形瓶中,收集滤液到40-50ml,盖上塞子,剧烈振荡2min,在室温下静置30分钟。取10mL滤液进行氮吹浓缩,温度35℃,浓缩至近干,定容到4ml,进GPC净化,GPC净化时,因为满环进样才2mL,所以进样也就是2ml,分段收集洗脱液,氮吹浓缩至近干,温度也是35℃,最后定容至2mL,GC-MS上样分析。我用的是外标法,标样浓度分别为0.1,0.3,0.5.0.7,1.0.最后根据标准曲线求出C。

我的计算公式是:试样中农药的含量X (mg/kg)= C×2×2×10×1000/ m×50×1000,麻烦大家帮我看一看计算公式对不对。另外,我按照这个方法做加标回收,加标量为4ml (浓度为1ug/ml),最后计算的时候,敌敌畏和甲拌磷的回收率不到60%.麻烦大家做过的给我提点意见,十分感谢!
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