HPLC法测定碱水粑中的脱氢乙酸

Determination of Dehydroacetic Acid in Alkaline Water Cake by HPLC

建立一种快速检测碱水粑中脱氢乙酸含量的高效液相色谱方法。方法:称取5 g样品,经10%乙醇溶液提取、硫酸锌溶液+氢氧化钠溶液沉淀蛋白质,定容至25 mL,高速离心后取上层清液过滤膜,经高效液相色谱仪在293 nm检测波长下进行检测。结果:脱氢乙酸浓度在1.00~200.00 μg·mL^(-1)时与峰面积呈现良好的线性关系,相关系数R^(2)=0.999 8;方法检出限为0.001 3 g·kg^(-1),定量限为0.004 g·kg^(-1);经方法学验证结果表明,加标回收率为92.42%~98.65%,相对标准偏差为1.32%~2.50%。结论:本方法能够快速且准确地检测出碱水粑中脱氢乙酸的含量,适合在基层检验检测机构推广普及,具有一定的实际应用价值。

A high performance liquid chromatography method for dehydroacetic acid in alkaline water was established.Method:5 g of samples were weighed,extracted by 10% ethanol solution,zinc sulfate solution+sodium hydroxide solution,and settled to 25 mL.After centrifugation,the supernatwas filtered and tested at 293 nm by high-performance liquid chromatography.Result:Dehydroacetic acid concentration was from 1.00 to 200.00 μg·mL^(-1),the correlation coefficient R^(2)=0.999 8,the detection limit of the method was 0.001 3 g·kg^(-1),the quantification limit was 0.004 g·kg^(-1);the recovery rate was 92.42%~98.65% and relative standard deviation was 1.32%~2.50%.Conclusion:This method can quickly and accurately detect the content of dehydroacetic acid in the alkaline water cake,which is suitable for the popularization in the basic inspection and testing institutions,and has certain practical application value.