水蒸气蒸馏分离-高效液相色谱法测定烟用香精和料液中的6种防腐剂成分

Determination of Six Preservatives in Tobacco Flavor and Sauce by Steam Distillation Separation and High Performance Liquid Chromatography

建立高效液相色谱法同时测定烟用香精和料液中6种常见防腐剂(苯甲酸,山梨酸,脱氢乙酸,对羟基苯甲酸甲酯、乙酯、丙酯)的检测方法。样品在磷酸和饱和硫酸铵介质中水蒸气蒸馏分离,然后再用Waters Oasis HLB反相固相萃取净化。以甲醇和0.1%的甲酸溶液为流动相梯度洗脱,采用二极管阵列检测器检测。结果显示,6种组分分离完全,线性良好,加标回收率为93%~104%,日内相对标准偏差为1.8%~2.6%,日间相对标准偏差为2.1%~3.0%。该方法灵敏度高、选择性好、回收率高、简单快捷,能满足烟用香精和料液样品中6种防腐剂成分检测的要求。

A new method for the simultaneous determination of six preservatives （benzoic acid, sorbic acid, dehydrogenation acid, methyl-p-hydroxybenzoate, ethyl-p-hydrnxybenzoate, and propyl-p-hydroxy benzoate） in tobacco flavor and sauce by high performance liquid chromatography （HPLC） was developed. The preservatives were separated by steam distillation in phosphoric acid and saturated ammonium sulfate medium, and then purified by reverse phase solid phase extraction with Waters Oasis HLB cartridge. The six preservatives were separated by HPLC with methanol and 0.1% formic acid gradient elution as mobile phase, and detected with diode array detector. The results showed that the six preservatives were separated completely and the linearity was good. The recoveries of six preservatives were ranged from 93 % - 104 %. The intraday relative standard deviations were ranged from 1.8 % - 2.6 %, and the interday relative standard deviation were ranged from 2.1% - 3 %. This method is high sensitivity, good selectivity, high recovery rates, simple, and quick, and can meet the requirement of six kinds of preservatives in tobacco flavor and sauce samples with good results.