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RP-HPLC法测定烟用香精香料中的7种防腐剂

Determination of Seven Preservatives in Tobacco Flavor by RP-HPLC

  • 摘要: 为了测定烟用香精香料中的防腐剂,考察了萃取条件、色谱分离条件和检测条件对测定结果的影响,建立了同时测定烟用香精香料中7种防腐剂的方法,并采用该方法检测了9种烟用香精香料中的防腐剂。结果表明:①用甲醇超声提取5 min效果较好;②用Dikma Platisil ODS色谱柱,甲醇和水(调节pH值)为流动相,梯度洗脱,流速1.0 mL/min,40 min内7种防腐剂达到完全分离;③分时段在10 min前采用230 nm波长检测苯甲酸、水杨酸、山梨酸,在10min后在254 nm波长处检测苯甲酸酯类,灵敏度高;④该法的回收率为97.0%~99.6%,5次重复实验的RSD范围为1.3%~3.1%,均小于5%;⑤除8号样品外,其他样品中均添加有防腐剂,主要是苯甲酸和山梨酸,有3种样品中测出了对羟基苯甲酸酯类,水杨酸均未检出。该方法适合烟用香精香料中的7种防腐剂的检测。

     

    Abstract: A method for simultaneously determining 7 preservatives in tobacco flavors by reversed-phase high performance liquid chromatography(RP-HPLC) with a variable wavelength detector(VWD) was developed.The parameters such as extraction solvent,extraction time,mobile phase,VWD wavelength were tested and optimized.The preservatives in 9 tobacco flavor samples were quantitatively determined respectively,the results showed that:① ultrasonic extraction with methanol for 5 min was more effective;② the 7 preservatives were completely separated in 40 min by reversed-phase HPLC with a Dikma Platisil ODS column under a gradient elution with methanol and water(adjusted pH) as mobile phase at a flow-rate of 1.0 mL/min;③ at a wavelength of 230 nm in the first 10 min to detect benzoic acid,salicylic acid,sorbic acid,then at 254 nm to detect esters of methyl parabenzoic acid presented higher sensitivity;④ the recoveries of preservatives were from 97.0% to 99.6% with the relative standard deviation(RSD) of 5 repeat tests under 5%(1.3%-3.1%);⑤ none of the preservatives was found in Sample No.8,the preservatives detectable in the other samples mainly were benzoic acid and sorbic acid,esters of methyl parabenzoic acid were found in 3 samples and salicylic acid was not detected in all samples.This method is suitable for determining the 7 preservatives in tobacco flavors.

     

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