Longares-Patrón Arturo, Cañizares-Macías M P
Department of Analytical Chemistry, Faculty of Chemistry, Universidad Nacional Autónoma de México (UNAM), 04510 México D.F., Mexico.
Talanta. 2006 Jun 15;69(4):882-7. doi: 10.1016/j.talanta.2005.11.030. Epub 2005 Dec 13.
A new method to quick extraction of vanillin and p-hydroxybenzaldheyde (PHB) of vanilla beans from vanilla fragans is proposed. Samples were irradiated with microwaves energy to accelerate the extraction process and photometric monitoring was performed at 348 and 329nm (vanillin and PHB, respectively). The simultaneous determination of vanillin and PHB from extracts was performed using the Vierordt's method, which showed a precision, expressed as relative standard deviation, smaller 2.5% for both analytes. Conditions such as microwaves irradiation power, number of irradiation and non-irradiation cycles, irradiation time and ethanol concentration were optimized by means of multivariate screening that showed that irradiation power and number of irradiation cycles are the most significant condition in the vanilla extraction process. The focused microwave-assisted extraction (FMAE) was applied to commercial (dried vanilla beans from fresh green vanilla beans), lyophilised and dried (commercial vanilla dried at 135 degrees C in oven) vanilla beans samples. The results showed that the extraction of vanillin and PHB in the commercial vanilla samples were higher than in dried and lyophilised samples. With the proposed FMAE a decrease in the extraction time of 62 times and an increase in the vanillin and PHB concentrations between 40 and 50% with respect to the official Mexican extraction method, were obtained.
提出了一种从香荚兰中快速提取香兰素和对羟基苯甲醛(PHB)的新方法。用微波能量辐照样品以加速提取过程,并分别在348nm和329nm(香兰素和PHB)处进行光度监测。使用Vierordt法对提取物中的香兰素和PHB进行同时测定,结果表明,两种分析物的精密度(以相对标准偏差表示)均小于2.5%。通过多变量筛选对微波辐照功率、辐照和非辐照循环次数、辐照时间和乙醇浓度等条件进行了优化,结果表明辐照功率和辐照循环次数是香荚兰提取过程中最显著的条件。聚焦微波辅助萃取(FMAE)应用于商业样品(由新鲜绿色香荚兰豆干燥而成)、冻干和干燥(在135℃烘箱中干燥的商业香荚兰)香荚兰豆样品。结果表明,商业香荚兰样品中香兰素和PHB的提取量高于干燥和冻干样品。与墨西哥官方提取方法相比,采用所提出的FMAE可使提取时间减少62倍,香兰素和PHB浓度提高40%至50%。