评估易于使用的样品处理策略的潜力:膳食补充剂中典型成分的 "摩卡提取 "多变量研究

IF 5.2 Q1 CHEMISTRY, ANALYTICAL Advances in Sample Preparation Pub Date : 2024-03-11 DOI:10.1016/j.sampre.2024.100110
Matteo Baglietto, Barbara Benedetti, Marina Di Carro, Emanuele Magi
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摘要

Bialetti 先生于 1933 年发明了摩卡咖啡机,至今仍是家庭烹制咖啡最常用的方法。摩卡咖啡机从咖啡粉中提取成分的过程是在高压和高温下进行的固液萃取。在简单的样品处理策略中,这些特性是非常理想的,因为它们能在短时间内实现良好的萃取效率。本文首次将摩卡壶萃取作为从膳食补充剂中萃取极性化合物的替代处理方案。通过对集合基质进行分因子实验设计,评估了四个实验变量对提取效率的影响。特别是考虑了溶剂的 pH 值及其有机改性剂的含量、加热温度和样品质量(反映了与溶剂量的比例,由于实际需要,溶剂量必须保持固定)。然后,通过测定不含任何目标分析物的加标基质的回收率(介于 52% 与 134% 之间,乙酰水杨酸除外)和基质效应(稀释 100 倍后始终可忽略或适度),验证了最佳条件的性能。最后,将这些方法应用于实际样品,对人工甜味剂、甲基黄嘌呤和牛磺酸等化合物进行了定量分析。然后将结果与标签上标注的数量以及之前开发的盐辅助液液萃取法(SALLE)得出的结果进行比较。有趣的是,这两种方法对大多数化合物的提取效果相当,但摩卡萃取法可以对牛磺酸进行定量,而盐辅助液液萃取法则无法回收牛磺酸。这一令人鼓舞的结果激励着我们进一步开展工作,将简单的 Moka 设备的应用扩展到其他分析物和更多基质。
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Assessing the potentialities of an easy-to-use sample treatment strategy: Multivariate investigation on “Moka extraction” of typical ingredients from dietary supplements

Mr. Bialetti invented Moka in 1933 and it still represents the most common way to prepare coffee at home. The process through which Mokas extract components from the ground coffee is a solid-liquid extraction which occurs at high pressure and temperature. These features are desirable in simple sample treatment strategies, since they allow good extraction efficiencies in a short time. Herein, for the first time, Moka-pot extraction was considered as an alternative processing protocol to extract polar compounds from dietary supplements. The effect of four experimental variables on extraction efficiency was evaluated through a fractional factorial design of experiments applied to a pooled matrix. In particular, solvent pH and its content of organic modifier, heating temperature and sample mass (reflecting the ratio to the amount of solvent which has to be kept fixed due to practical needs) were considered. The performances of the best conditions were then validated by determining recoveries (between 52 and 134 %, except for acetylsalicylic acid) and matrix effects (resulting always negligible or moderate at 100-fold dilution) of a spiked matrix which did not present any of the target analytes. They were finally applied to real samples, allowing to quantify some compounds, including artificial sweeteners, methylxanthines and taurine. Results were then compared with the quantities declared on the labels and those obtained with a Salt-Assisted Liquid-Liquid Extraction (SALLE), previously developed. Interestingly, the two methods were comparable for most compounds, but Moka extraction allowed to quantify taurine, which was not recovered with the SALLE. This promising result encourages further work to extend the use of the simple Moka device to other analytes and further matrices.

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