精甲霜灵柱层析净化淋洗液的改进研究

精甲霜灵为外消旋物甲霜灵的R型对映体,其在农产品中的残留分析方法中多采用活性等级Ⅴ的酸性氧化铝填充柱并用正己烷与乙醚的混合淋洗液淋洗净化。但由于乙醚有较强刺激性,对实验人员危害较大。经试验,改用正已烷:二氯甲烷(1∶1)的混合淋洗液淋洗,其添加回收率可达95.39%,标准分离值为4.10,变异系数为4.30%,经SA S系统方差分析两者间无差异。精甲霜灵与其荔枝果肉添加样品中的杂质峰最小分离度R为1.668,与相邻组分能完全分离。

Modification on purified eluting solution of metalaxyl-M column Chromatography

Metalaxyl-M is a (R)-enantiomer of racemate metalaxyl,and is mostly eluted with n-hexane and diethyl ether mixed eluting solution in analysis of residues in agricultural products by applying acidic alumina (active grade V) chromatographic column. In order to avoid the pungency of diethyl ether and ensure safety to the workers on operation,a mixed solution of n-hexane and dichloromethane (1∶1) was used as a substitute of diethyl ether in the present study. The average additive recovery percentage in the control specimen of litchi flesh was 95.39% with standard deviation 4.10 and coefficient of variation 4.30%,which was not significantly different from the results analyzed with the mixed solution of n-hexane and diethyl ether. With the new method,the minimal resolution (R) of impurity peak was 1.668,and the adjacent components could be separated completely.