用薄层色谱和高效液相色谱- pda分析香兰药材和酊剂中香兰素的含量

M. Ferreira, M. Schwanz, G. Cosenza, A. Henriques, L. Soares
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摘要

planifolia香草planifolia(兰科)是一个享誉全球的物种,是食品、化妆品和制药行业中使用的香草素香料的最大来源。采用薄层色谱(TLC)和高效液相色谱(HPLC-PDA)对平叶草中草药和酊剂中香兰素的含量进行了分析。用氢化酒精溶液回流制得中药;薄层色谱法对反应进行动力学分析。通过实验设计,研究了溶剂和药液浓度的影响。分别制备中草药、酊剂和标准香兰素溶液,采用高效液相色谱(HPLC)和DAD检测器(波长280 nm)进行分析。以1.0 g草药料和50%乙醇(v/v)为溶剂,经过3次提取循环得到香兰素的总提取率。该方法具有良好的重复性(RSD < 0.90)、中间精密度(RSD < 1.09)、回收率(93.12 ~ 113.74%)和鲁棒性(RSD < 4.33)。草药和酊剂中香兰素的总含量分别为1.82 g%和0.21 g%。一种简单、优化的反流制样方法能够全面提取香兰素,且不影响HPLC-PDA方法的可靠性。验证了色谱法分离和定量平叶豆荚中草药和酊剂中香兰素的方法。
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ANALYSIS OF VANILLIN BY TLC AND HPLC-PDA IN HERBAL MATERIAL AND TINCTURE FROM Vanilla planifolia Jacks ex. Andrews
Vanilla planifolia (Orchidiaceae) is a species that is renowned globally and represents the largest source of vanillin flavoring used in the food, cosmetic and pharmaceutical industries. This study was carried out to analyze by TLC and HPLC-PDA vanillin in herbal drug and tincture from V. planifolia. The herbal drug was obtained with hydroalcoholic solution under reflux; and a kinetic reaction was performed by TLC. The influences of solvent and herbal drug concentration were studied through an experimental design. The solutions (herbal drug, tincture and standard – vanillin) were prepared and analyzed in HPLC coupled with DAD detector, using wavelength of 280 nm. The total extraction of vanillin was achieved after three extraction cycles, using 1.0 g of herbal material and Ethanol 50% (v/v) as solvent. The method was linear (R2> 0.99) and demonstrated repeatability (RSD < 0.90), intermediate precision (RSD < 1.09), recovery (93.12-113.74%), as well as robustness (RSD < 4.33). The total content of vanillin found was 1.82 g% and 0.21 g% for herbal drug and tincture, respectively. A simple and optimized method for sample preparation by reflux was able to provide the exhaustive extraction of vanillin and does not compromise the reliability of the HPLC-PDA method. The chromatographic procedure was validated to separate and quantify vanillin in herbal material and tincture from pods of V. planifolia.
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