Comparison of critical methods developed for fatty acid analysis: A review

Wu, Zhuona; Zhang, Qi; Li, Ning; Pu, Yang; Bing, Wang; Zhang, Tong

doi:10.1002/jssc.201600707

Cited by 32 publications

(21 citation statements)

References 85 publications

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“…In fact, if the detection of olive oil frauds and quality assurance is generally still a difficult issue that requires several improvements, [4] the authentication of PDO VOOs is an additional challenge. [30][31][32] Moreover, other analytical techniques based on chromatographic approaches have also been employed to identify and quantify major and many minor oil components. [24] The quality of PDO VOOs has been evaluated using different wet methods, such as the determination of free fatty acids, [25][26][27][28] specific extinction coefficients (K 232 and K 270), [26,27,29] peroxide value, [26,27,29] or anisidine value.…”

Section: Control Tools To Authenticate Pdo Voosmentioning

confidence: 99%

“…The quality of PDO VOOs has been evaluated using different wet methods, such as the determination of free fatty acids, specific extinction coefficients (K 232 and K 270), peroxide value, or anisidine value . However, these methods are generally laborious and time consuming, require the use of several solvents and reagents, and only provide information about certain parameters, included in the legal norms, that make reference to the concentration of non desirable compounds in the oil …”

Section: Control Tools To Authenticate Pdo Voosmentioning

confidence: 99%

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Potential of Nuclear Magnetic Resonance for a Discriminant Characterization of PDO VOOs

Caño-Ochoa

Ruiz‐Aracama

Loren

2018

Euro J Lipid Sci & Tech

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Interest in virgin olive oil (VOO) is growing among consumers and industry due to its well‐received sensorial attributes and to its higher oxidative stability, as well as to its positive health effects. Furthermore, attention is being increasingly paid to other quality attributes of VOO, such as sustainability and geographical origin. For these reasons, this oil has an important added value and is exposed to fraudulent practices. In order to guarantee its origin, the European Union (EU) has developed the Protected Designation of Origin (PDO) quality scheme that links the characteristics of a VOO to its geographical origin. In recent years attempts to develop tools that enable the authentication of PDO‐labeled VOOs are carried out. In this regard, studies using Nuclear Magnetic Resonance (NMR) to this aim are here reviewed. Practical Applications: Due to the added value of PDO VOOs, their authentication is of great importance for administration, consumers and producers. The studies in which NMR spectroscopy has been used to this aim are analyzed here. In this context, this review provides a view of the state of the art that can be of practical interest not only for the researchers of the subject but also for the aforementioned groups. Approaches based on NMR spectroscopic data combined with different statistical analysis are used to develop predictive models with the aim of discriminating PDO VOOs from non‐PDO oils, or even to discriminate a VOO from a certain PDO from other different PDO oils.

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Section: Control Tools To Authenticate Pdo Voosmentioning

confidence: 99%

Section: Control Tools To Authenticate Pdo Voosmentioning

confidence: 99%

Potential of Nuclear Magnetic Resonance for a Discriminant Characterization of PDO VOOs

Caño-Ochoa

Ruiz‐Aracama

Loren

2018

Euro J Lipid Sci & Tech

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“…Change in shift and/or the integration area of the proton signals can provide information about degradation mechanism, especially ester hydrolysis of PS. 9,10,11,12 Verbrugghe et al used dif-fusion ordered 1 H NMR to quantify non-esterified ethoxylates in PS surfactants. This is important since these do not contribute to stabilisation of therapeutic proteins.…”

Section: Introductionmentioning

confidence: 99%

Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input Polysorbates

Brovč

Pajk

Šink³

et al. 2019

ACSi

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Polysorbates (PS) are the most common non-ionic surfactants used in protein formulations. Their degradation has been studied intensively in recent years. Ester bond hydrolysis is one of many pathways of PS degradation that can lead to accumulation of free fatty acids (FFAs) and particle formation. The distribution and quantity of FFAs in PSs impacts directly on product quality. Characterization of input PS is highly relevant, because the initial content of FFAs differs greatly between manufacturers. The purpose of this study was to set up a quick and simple analytical method for the quantitative evaluation of FFAs in PS. The content of FFAs was measured for selected PS 20 and 80, using two methods, 1 H nuclear magnetic resonance spectroscopy (1 H NMR) and the European pharmacopoeia method for determining acid value (I A). These methods have been evaluated using the method of standard addition and, based on the results, they are interchangeable. It was concluded that 1 H NMR is a useful tool for quality control of input PS and a rapid method for indicating the rate of PS degradation by hydrolysis and oxidation. Further, a newly discovered impurity in PS raw material, the long chain ketone 12-tricosanone, can be identified using 1 H NMR.

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“…A great advantage of HPLC methods over GC methods is that the eluted FAs are not destroyed during their detection. So, HPLC methods make possible the collection of desired fractions of FAs for further analysis (Lima and Abdalla 2002;Ruiz-Rodriguez et al 2010;Wang et al 2009;Wu et al 2016). HPLC methods also enable the lower temperature application during analysis, which reduces the risk of isomerization of unsaturated FAs, and they offer the advantages of speed, resolution, high sensitivity, and specificity (Obert et al 2007;Funazo et al 1989).…”

Section: Introductionmentioning

confidence: 99%

“…Due to the chemical characteristics of FAs, the majority of FA derivative separations by HPLC are reverse-phase (RP) systems. In RP-HPLC mode, both the retention and the selectivity increase as the alkyl chain of the bonded phase is lengthened (Wu et al 2016;Mansour 2005;Christie et al 2007). In addition to RP-HPLC, other modes of liquid chromatography such as argentation (Ag + -HPLC) and ion-pair liquid chromatography (IP-HPLC) have also been widely applied for the analysis of specific FAs (Winkler and Steinhart 2001;Adlof 2004;Villegas et al 2010;Delmonte et al 2008;Tsuyama et al 1992).…”

Section: Introductionmentioning

confidence: 99%

Application of Central Composite Design for the Optimization of Reverse-Phase HPLC/DAD Separation of the cis- and trans- Isomers of Long-Chain Unsaturated Fatty Acids

Arslan

Azak

2017

Food Anal. Methods

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The study deals with the optimization of reversephase HPLC separation of cis-/transisomers of long-chain unsaturated fatty acids by the assessment of the central composite design (CCD) of response surface methodology (RSM). The optimized conditions were also applied for the analysis of fatty acids in functional cold-pressed oils. The data obtained from experimental applications of CCD was used to model the parameters that significantly affect separations. The independent variables chosen were flow rate (X 1), column temperature (X 2), and acetonitrile content in mobile phase (X 3). A second-order polynomial model was used to estimate the impact of variables on separation efficiencies of the C30 and C18 stationary phases. The proposed CCD models were also validated with the ANOVA. The predicted values were in good agreement with experimental data, advising expert application of CCD as an option to obtain maximum information for the modeling of reverse-phase HPLC separation with little number of experiments. The optimal values of method parameters for the efficient C18 and C30 column separations as part of the k′ response value were found to be flow rate of 1.10 and 0.42 mL min −1 , temperature of 3.6 and 9.4°C, and acetonitrile content in mobile phase of 100 and 77.4%, respectively. ANOVA test results also illustrate that the CCD models can be successfully used to predict the optimum method parameters. To maximize both sensitivity and precision of the methods, the validation procedure was also performed and the higher correlation coefficients (r = 0.9149-0.9993) were determined for all fatty acid methyl esters. Thus, the proposed experimental designs were shown to offer considerable advantages over traditional method optimization approaches.

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Comparison of critical methods developed for fatty acid analysis: A review

Cited by 32 publications

References 85 publications

Potential of Nuclear Magnetic Resonance for a Discriminant Characterization of PDO VOOs

Potential of Nuclear Magnetic Resonance for a Discriminant Characterization of PDO VOOs

Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input Polysorbates

Application of Central Composite Design for the Optimization of Reverse-Phase HPLC/DAD Separation of the cis- and trans- Isomers of Long-Chain Unsaturated Fatty Acids

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