scholarly journals Pattern-Type Separation of Triacylglycerols by Silver Thiolate×Non-Aqueous Reversed Phase Comprehensive Liquid Chromatography

Separations ◽  
2021 ◽  
Vol 8 (6) ◽  
pp. 88
Author(s):  
Paola Arena ◽  
Danilo Sciarrone ◽  
Paola Dugo ◽  
Paola Donato ◽  
Luigi Mondello

Triacylglycerols (TAGs), as the main components of edible oils and animal fats, are responsible for the nutritional value, organoleptic features and technological properties of foods; each lipid matrix shows a unique TAG profile which can serve as fingerprint to ensure the quality and authenticity of food products. The high complexity of many foodstuffs often makes untargeted elucidation of TAG components a challenging task; thus, more efficient separation techniques may be mandatory. In this research, the TAG profile of a borage (Borago officinalis) seed oil was obtained by two-dimensional comprehensive liquid chromatography (LC×LC), by the coupling of silver thiolate and octadecylsilica monodisperse materials. A total 94 TAG compounds were identified by ion trap-time of flight detection, using atmospheric pressure ionization, with the degree of unsaturation varying from 0 to 9, and partition values ranging from 36 to 56. The group-type separation afforded by this analytical approach may be useful to quickly fingerprint TAG components of oil samples.

The constitution of the hydrocarbon fraction has been determined by gas/liquid chromatography. Ten alkanes containing both odd and even numbers of carbon atoms have been found. Nonacosane (93 %) and hentriacontane (3 %) are the main components. The constitution of the nonacosane derivatives has been elucidated by subjecting each fraction to modified Baeyer-Villiger oxidation and identifying the key fragments by a combination of adsorption and reversed-phase partition chromatography on films of adsorbent supported on glass plates. A pair of isomers has been found in each group. Those from the ketone and secondary alcohol are derived by substitution of oxygen atoms in the 10- and 15-positions. In the ketol the oxygen substituents are also in the 10- and 15-positions and the isomers are derived by interchanging the positions of the hydroxyl and carbonyl groups.


2003 ◽  
Vol 86 (3) ◽  
pp. 612-622 ◽  
Author(s):  
Jitka Zrostlíková ◽  
Jana Hajšlová ◽  
Tomáš Kovalczuk ◽  
Radim Štěpán ◽  
Jan Poustka

Abstract A simple liquid chromatography/mass spectrome-try (LC/MS) approach for the determination of widely used representatives of polar/thermolabile pesticides in fruits was developed and validated. The group of pesticides comprised benzimidazoles and azoles (carbendazim, thiabendazole, imazalil, propiconazole, prochloraz, epoxiconazole, flusilazole, tebuconazole, bitertanol); N-methylcarbamates (carbaryl, carbofuran, methiocarb); and phenylureas and benzoylphenylureas (linuron, diflubenzuron, triflumuron, teflubenzuron, flufenoxuron). Matrixes (apple, apricot) were extracted with acetonitrile and crude extracts were cleaned up by solid-phase ex-traction (SPE) using either mixed cation exchange or hydrophilic lipophilic balance cartridges. LC separation of pesticides was performed on a reversed-phase column, Discovery C18. Electrospray ionization and ion trap MS/MS detection were applied. For most pesticides, overall recoveries ranged from 75 to 122%, and repeatability (as relative standard deviation) from 5 repetitive determinations of recovery ranged from 3 to 21%. Carbofuran was the only compound for which recovery was not satisfactory due to its loss in the SPE cleanup step. Limits of detection were 0.1–3 μg/kg for benzimidazole and azole fungicides and carbamate insecticides. For urea insecticides, detection limits were slightly higher (3–10 μg/kg).


OCL ◽  
2020 ◽  
Vol 27 ◽  
pp. 26
Author(s):  
Kamilia Kemel ◽  
Danielle Libong ◽  
Audrey Solgadi ◽  
Sana Tfaili ◽  
Arlette Baillet-Guffroy ◽  
...  

Linoleoyl macrogolglyceride (LM) and oleoyl macrogolglyceride (OM) are pharmaceutical ingredients, obtained from corn and apricot kernel oils respectively. This study aims to know the detailed chemical composition of LM and OM, in order to understand their roles in pharmaceutical formulations. These two products were analyzed by non-aqueous reversed phase high-performance liquid chromatography (NARP-HPLC), using Vintage Series KR C18 column (250 × 4.6 mm, 5 µm) and non-aqueous acetonitrile/acetone mixture as mobile phase. The ionization source used was atmospheric pressure photoionization (APPI) and the analyzer was LTQ-Orbitrap® (hybrid analyzer: double linear ion trap coupled to a Fourier transform orbital trap). LM and OM consist of complex mixtures, constituted of mono-(MG), di-(DG) and triglycerides (TG) and mono-(MPEGE) and di PEG-6 esters (DPEGE) of linoleic acid (18:2) for LM and of oleic acid (18:1) for OM. NARP-HPLC-APPI method allowed the separation and the identification of the glyceride classes (MGs, DGs and TGs) and the PEG esters of different chain lengths (PEG-chain lengths of fatty acid moieties and number of units of ethylene oxide), at the same time and in one single run, for both products LM and OM. The comparative study between LM and OM showed that, a higher presence of linoleic esters for LM, and a higher presence of oleic esters for OM.


1984 ◽  
Vol 62 (5) ◽  
pp. 301-309 ◽  
Author(s):  
S. Pind ◽  
A. Kuksis ◽  
J. J. Myher ◽  
L. Marai

The sn-1,2-diacylglycerol moieties of natural phosphatidylcholines as the tertiary-butyldimethylsilyl ethers were resolved on the basis of their carbon number and degree of unsaturation by high pressure liquid chromatography on reversed-phase C18 columns. Using acetonitrile and propionitrile as eluting solvents and reagent gases, the yields of both quasi molecular and fragment ions were found to vary with the degree of unsaturation and positional distribution of the fatty acids in the diacylglycerol molecules, and appropriate calibration factors were necessary for accurate quantitation. In the absence of pure structural isomer and mixed acid standards, we have determined preliminary calibration factors for total and specific ion current responses, by comparing the peak area ratios obtained by liquid chromatography – mass spectrometry with the weight and mole proportions of molecular species known to be present in the samples from detailed analyses by capillary gas–liquid chromatography on polar liquid phases. It was found that the total chemical ionization current response agreed closely with the weight composition of the molecular species. The relative yields of the (MH – 132)+ ions varied over one- to three-fold, while those of the (MH – RCOOH)+ ions varied over a three- to four-fold range of intensities. After suitable calibration of the relative ion response, it was possible to determine the identity and quantity of all common molecular species in the test diacylglycerophospholipids. Although the derived factors include both chromatographic and mass spectrometrie effects and are obtained with a gradient of reagent gases, they appear to be generally applicable.


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