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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。
To establish a method for simultaneous determination of six common preservatives (benzoic acid, sorbic acid, dehydroacetic acid, methylparaben, ethyl ester, propyl ester) in tobacco flavor and feedstock by HPLC. The sample was steam distilled in a mixture of phosphoric acid and saturated ammonium sulfate and then purified by reverse phase SPE with Waters Oasis HLB. Methanol and 0.1% formic acid solution as the mobile phase gradient elution, using a diode array detector test. The results showed that the six components were separated completely and the linearity was good. The recoveries were 93% -104%. The relative standard deviations were 1.8% -2.6%. The relative standard deviations were 2.1% -3.0%. The method has the advantages of high sensitivity, good selectivity, high recovery rate, simple and quickness, and can meet the requirements of testing six preservative components in tobacco flavor and liquid samples.