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采用毛细管电泳法测定橄榄油酸度。

Determination of olive oil acidity by CE.

作者信息

Balesteros Manoela R, Tavares Marina F M, Ribeiro Sidney J L, Polachini Ferminio C, Messaddeq Younes, de Oliveira Marcone A L

机构信息

Departamento de Química, Universidade Federal de Juiz de Fora, Juiz de Fora, MG, Brasil.

出版信息

Electrophoresis. 2007 Oct;28(20):3731-6. doi: 10.1002/elps.200700507.

Abstract

In this work, a CE method for the determination of olive oil acidity was proposed. The method was based on an ethanolic extraction (at 60 degrees C) of the oil long-chain free fatty acids (LC-FFAs) components followed by CE determination in pH 6.86 phosphate buffer at 15 mmol/L concentration containing 4 mmol/L sodium dodecylbenzenesulfonate (SDBS), 10 mmol/L polyoxyethylene 23 lauryl ether (Brij 35), 2% v/v 1-octanol and 45% v/v ACN under indirect UV detection at 224 nm. Although this electrolyte promoted baseline separation of myristic acid (C14:0) (internal standard (IS)) and olive oil major components (palmitic acid (C16:0), oleic acid (C18:1c) and linoleic acid (C18:2cc)) in less than 8 min, after a few injections, the electropherogram profiles were severely altered (peak broadening, migration time shifts, etc.) and the current increased substantially. An adsorption study was conducted revealing that the dissolution of the capillary external polyimide coating during the electrophoretic run caused the detrimental effect. After removal of the capillary tip coating, ten consecutive injections could be performed without any disturbances and this simple procedure was, therefore, implemented during quantitative purposes. The reliability of the proposed method was further investigated by the determination of acidity of an extra virgin olive oil sample in comparison to the established methodology (AOCS method Ca 5a-40, alkaline volumetric titration (AVT)). No statistical differences were found within 95% confidence level. A % acidity of 0.39 +/- 0.02 was found for the olive oil sample under consideration.

摘要

本研究提出了一种用于测定橄榄油酸度的毛细管电泳(CE)方法。该方法基于在60℃下用乙醇萃取油中的长链游离脂肪酸(LC - FFAs)成分,然后在15 mmol/L浓度、pH 6.86的磷酸盐缓冲液中进行CE测定,该缓冲液含有4 mmol/L十二烷基苯磺酸钠(SDBS)、10 mmol/L聚氧乙烯23月桂醚(Brij 35)、2%(v/v)1 - 辛醇和45%(v/v)乙腈,在224 nm处进行间接紫外检测。尽管这种电解质能在不到8分钟的时间内实现肉豆蔻酸(C14:0)(内标(IS))与橄榄油主要成分(棕榈酸(C16:0)、油酸(C18:1c)和亚油酸(C18:2cc))的基线分离,但经过几次进样后,电泳图谱严重改变(峰展宽、迁移时间偏移等),电流大幅增加。一项吸附研究表明,电泳过程中毛细管外部聚酰亚胺涂层的溶解导致了这种有害影响。去除毛细管尖端涂层后,可以连续进行十次进样而无任何干扰,因此,在定量分析时采用了这个简单的步骤。通过测定特级初榨橄榄油样品的酸度,并与既定方法(AOCS方法Ca 5a - 40,碱量滴定法(AVT))进行比较,进一步研究了所提方法的可靠性。在95%置信水平内未发现统计学差异。所研究的橄榄油样品的酸度为0.39±0.02%。

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