scholarly journals Rapid quantification of fatty acids in plant oils and biological samples by LC-MS

Author(s):  
Elisabeth Koch ◽  
Michelle Wiebel ◽  
Carolin Hopmann ◽  
Nadja Kampschulte ◽  
Nils Helge Schebb

AbstractAnalysis of fatty acids (FA) in food and biological samples such as blood is indispensable in modern life sciences. We developed a rapid, sensitive and comprehensive method for the quantification of 41 saturated and unsaturated fatty acids by means of LC-MS. Optimized chromatographic separation of isobaric analytes was carried out on a C8 reversed phase analytical column (100 × 2.1 mm, 2.6 μm core–shell particle) with a total run time of 15 min with back pressure lower than 300 bar. On an old triple quadrupole instrument (3200, AB Sciex), pseudo selected reaction monitoring mode was used for quantification of the poorly fragmenting FA, yielding limits of detection of 5–100 nM. Sample preparation was carried out by removal of phospholipids and triglycerides by solid-phase extraction (non-esterified fatty acids in oils) or saponification in iso-propanol (fatty acyls). This is not only a rapid strategy for quantification of fatty acyls, but allows the direct combination with the LC-MS-based analysis of fatty acid oxidation products (eicosanoids and other oxylipins) from the same sample. The concentrations of fatty acyls determined by means of LC-MS were consistent with those from GC-FID analysis demonstrating the accuracy of the developed method. Moreover, the method shows high precisions with a low intra-day (≤ 10% for almost all fatty acids in plasma and ≤ 15% in oils) and inter-day as well as inter-operator variability (< 20%). The method was successfully applied on human plasma and edible oils. The possibility to quantify non-esterified fatty acids in samples containing an excess of triacylglycerols and phospholipids is a major strength of the described approach allowing to gain new insights in the composition of biological samples. Graphical abstract

2021 ◽  
pp. 108201322199884
Author(s):  
Rami Akkad ◽  
Ereddad Kharraz ◽  
Jay Han ◽  
James D House ◽  
Jonathan M Curtis

The odour emitted from the high-tannin fab bean flour ( Vicia faba var. minor), was characterized by headspace solid-phase microextraction/gas chromatography-mass spectrometry (HS-SPME/GC–MS). The relative odour activity value (ROAV) was used to monitor the changes in key volatile compounds in the flour during short-term storage at different temperature conditions. The key flavour compounds of freshly milled flour included hexanal, octanal, nonanal, decanal, 3-methylbutanal, phenyl acetaldehyde, (E)-2-nonenal, 1-hexanol, phenyl ethyl alcohol, 1-octen-3-ol, β-linalool, acetic acid, octanoic acid, and 3-methylbutyric acid; these are oxidative degradation products of unsaturated fatty acids and amino acids. Despite the low lipid content of faba beans, the abundances of aldehydes arising during room temperature storage greatly contributed to the flavour of the flour due to their very low odour thresholds. Two of the key volatiles responsible for beany flavour in flour (hexanal, nonanal) increased greatly after 2 weeks of storage at room temperature or under refrigerated conditions. These volatile oxidation products may arise as a result of enzymatic activity on unsaturated fatty acids, and was seen to be arrested by freezing the flour.


1989 ◽  
Vol 120 (2) ◽  
pp. 175-179 ◽  
Author(s):  
C. Street ◽  
R. J. S. Howell ◽  
L. Perry ◽  
S. Al-Othman ◽  
T. Chard

Abstract. The effect of non-esterified fatty acids (NEFA) on the in vitro binding of testosterone, 5-alpha dihydrotestosterone and estradiol E2 to sex hormone binding globulin (SHBG) was examined using pooled normal female serum, and SHBG and albumin fractions obtained from the partial purification of late pregnancy serum. A range of saturated and unsaturated fatty acids were examined for their effect on steroid-protein binding. In normal female serum, NEFA added at physiological concentrations disrupted steroid-protein binding. The shorter chain (C8–C12) saturated acids and the poly-unsaturated acids proved to be more effective inhibitors than the longer chain saturated or mono-unsaturated acids. The greatest inhibition was obtained with E2 whereas the binding of dihydrotestosterone was least affected. With partially purified SHBG, the same concentrations of NEFA were less effective at inhibiting the binding of dihydrotestosterone and testosterone but elicited the same effect with E2. The binding of steroids to albumin appeared to be unaffected by these concentrations of NEFA.


1967 ◽  
Vol 45 (13) ◽  
pp. 1405-1410 ◽  
Author(s):  
John D. Castell ◽  
R. G. Ackman

The total acidic products from the performic acid oxidation of the ozonide of methyl oleate formed in methanol may be esterified directly in a few hours with 2,2-dimethoxypropane. The ester concentrations are adequate for the determination of the positional isomers of monoethylenic fatty acids directly from the reaction mixture, using a hydrogen flame ionization gas–liquid chromatography detector. Dimethyl sulfoxide was not required to prevent the breakdown of 2,2-dimethoxypropane under the conditions employed.


2016 ◽  
Vol 62 (2) ◽  
pp. 206-211 ◽  
Author(s):  
V.A. Akmurzina ◽  
E.E. Petryairina ◽  
S.V. Saveliev ◽  
A.A. Selishcheva

Composition and quantitative content of non-esterified fatty acids (NEFA) were investigated in plasma samples of healthy children (12) and children with type 1 diabetes mellitus (DM1) (31) by gas chromatography (GC) after preliminary NEFA solid-phase extraction from plasma lipids. There was a significant (p<0.001) 1.6-fold increase in the total level of NEFA regardless of the disease duration. In the group of DM1 children with the disease period less than 1 year there was an increase in the arachidonic acid (20:4) content (30%) and the oleic acid trans-isomer (18:1) content (82%), and also a decrease in the docosahexaenoic acid (22:6 n3) content (26% ) and the docosapentaenoic acids (22:5 n-6) content (60%). In the group of DM1 children with prolonged course of this disease the altered NEFA levels returned to the normal level


Nutrients ◽  
2020 ◽  
Vol 12 (5) ◽  
pp. 1232
Author(s):  
Agnieszka Stawarska ◽  
Małgorzata Jelińska ◽  
Julia Czaja ◽  
Ewelina Pacześniak ◽  
Barbara Bobrowska-Korczak

Fatty acids, especially polyunsaturated, and their metabolites (eicosanoids) play many pivotal roles in human body, influencing various physiological and pathological processes. The aim of the study was to evaluate the effect of supplementation with edible oils diverse in terms of fatty acid composition on fatty acid contents, activities of converting their enzymes, and on lipoxygenase metabolites of arachidonic and linoleic acids (eicosanoids) in rat serum. Female Sprague-Dawley rats divided into seven groups were used in the study. Animals from six groups were fed one of oils daily (carotino oil, made up by combining of red palm oil and canola oil, linseed oil, olive oil, rice oil, sesame oil, or sunflower oil). One group received a standard diet only. Fatty acids were determined using gas chromatography with flame ionization detection. Eicosanoids—hydroxyeicosatetraenoic (HETE) and hydroxyoctadecadienoic acids (HODE) were extracted using a solid-phase extraction method and analyzed with HPLC. Vegetable oils given daily to rats caused significant changes in serum fatty acid profile and eicosanoid concentrations. Significant differences were also found in desaturases’ activity, with the linseed and olive oil supplemented groups characterized by the highest D6D and D5D activity. These findings may play a significant role in various pathological states.


1980 ◽  
Vol 187 (3) ◽  
pp. 851-856 ◽  
Author(s):  
G Vallette ◽  
C Benassayag ◽  
L Savu ◽  
J Delorme ◽  
E A Nunez ◽  
...  

The novel endogenous serum ligands of rat alpha 1-foetoprotein previously demonstrated in different mammalian sera were identified by g.l.c.–mass-spectrometric methods as a mixture of non-esterified long-chain and predominantly unsaturated fatty acids. Detailed comparative analyses of these ligands extracted from foetal- and pregnant-rat sera, rat amniotic fluid and foetal human sera are presented. We also show that an important fraction of these ligands remains associated with the rat alpha 1-foetoprotein after purification; analyses are given for the composition of this lipid moiety of the foetoprotein. The physiological relevance of these results is discussed.


Molecules ◽  
2020 ◽  
Vol 25 (18) ◽  
pp. 4079 ◽  
Author(s):  
Jingnan Chen ◽  
Dami Li ◽  
Guiyun Tang ◽  
Jinfen Zhou ◽  
Wei Liu ◽  
...  

The stability of soybean germ phytosterols (SGPs) in different lipid matrixes, including soybean germ oil, olive oil, and lard, was studied at 120, 150, and 180 °C. Results on the loss rate demonstrated that SGPs were most stable in olive oil, followed by soybean germ oil, and lard in a decreasing order. It is most likely that unsaturated fatty acids could oxidize first, compete with consumption of oxygen, and then spare phytosterols from oxidation. The oxidation products of SGPS in non-oil and oil systems were also quantified. The results demonstrated that at relatively lower temperatures (120 and 150 °C), SGPs’ oxidation products were produced the most in the non-oil system, followed by lard, soybean germ oil, and olive oil. This was consistent with the loss rate pattern of SGPs. At a relatively higher temperature of 180 °C, the formation of SGPs’ oxidation products in soybean germ oil was quantitatively the same as that in lard, implying that the temperature became a dominative factor rather than the content of unsaturated fatty acids of lipid matrixes in the oxidation of SGPs.


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