采用反相液相色谱-紫外检测法快速测定香草提取物中香豆素、香草醛和乙基香草醛的方法。

Rapid method for the determination of coumarin, vanillin, and ethyl vanillin in vanilla extract by reversed-phase liquid chromatography with ultraviolet detection.

作者信息

Ali Laila, Perfetti Gracia, Diachenko Gregory

机构信息

U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, 5100 Paint Branch Pkwy, College Park, MD 20740, USA.

出版信息

J AOAC Int. 2008 Mar-Apr;91(2):383-6.

PMID:18476352

Abstract

A method is described for determining coumarin, vanillin, and ethyl vanillin in vanilla extract products. A product is diluted one-thousand-fold and then analyzed by reversed-phase liquid chromatography using a C18 column and a mobile phase consisting of 55% acetonitrile-45% aqueous acetic acid (1%) solution at a flow rate of 1.0 mL/min. Peaks are detected with a UV detector set at 275 nm. Vanilla extracts were spiked with 250, 500, and 1000 microg/g each of coumarin, vanillin, and ethyl vanillin. Recoveries averaged 97.4, 97.8, and 99.8% for coumarin, vanillin, and ethyl vanillin, respectively, with coefficient of variation values of 1.8, 1.3, and 1.3%, respectively. No significant difference was observed among the 3 spiking levels. A survey of 23 domestic and imported vanilla extract products was conducted using the method. None of the samples contained coumarin. The surveyed samples contained between 0.4 to 13.1 and 0.4 to 2.2 mg/g vanillin and ethyl vanillin, respectively.

摘要

描述了一种测定香草提取物产品中香豆素、香草醛和乙基香草醛的方法。将产品稀释1000倍，然后使用C18柱和由55%乙腈-45%乙酸水溶液（1%）组成的流动相，以1.0 mL/min的流速通过反相液相色谱进行分析。用设置在275 nm的紫外检测器检测峰。向香草提取物中分别加入250、500和1000 μg/g的香豆素、香草醛和乙基香草醛。香豆素、香草醛和乙基香草醛的回收率平均分别为97.4%、97.8%和99.8%，变异系数值分别为1.8%、1.3%和1.3%。在3个加标水平之间未观察到显著差异。使用该方法对23种国产和进口香草提取物产品进行了调查。所有样品均不含香豆素。被调查样品中香草醛和乙基香草醛的含量分别为0.4至13.1 mg/g和0.4至2.2 mg/g。