Comparison of the Determination of Eight Cholesterol Oxides in Dry–Cured Shoulder by GC–FID, GC–MS, and GC Tandem Mass Spectrometry

Abstract

The analysis of eight cholesterol oxidation products: 7α-hydroxycholesterol, 7β-hydroxycholesterol, α-epoxycholesterol, β-epoxycholesterol, 20α-hydroxycholesterol, cholestanetriol, 25-hydroxycholesterol, and 7-ketocholesterol in dry-cured shoulder was carried out. The extraction of lipids was performed by using the Bligh and Dyer method (1959). Interferences were removed by solid-phase extraction (SPE) in two steps with silica and aminipropylsilica SPE columns. The separation of the eight cholesterol oxidation products was done by gas chromatography, and the detection was performed by flame ionization detection (FID) and mass spectrometry (MS). The results obtained from the use of both systems of detection were compared. The results showed that gas chromatography-mass spectrometry (GC-MS) was the most suitable technique to obtain reliable quantitative data, and significant differences (p<0.05) between FID and MS determining 7α-hydroxycholesterol, 20α-hydroxycholesterol, and 25-hydroxycholesterol were observed. For the determination of cholesterol oxidation products, it was necessary to apply gas chromatography-tandem mass spectrometry to increase the sensitivity and to avoid interference from other compounds.

A review of analytical methods measuring lipid oxidation status in foods: a challenging task

“…GC-MS is the most accurate and commonly applied quantification method for this kind of compounds [62][63][64][65][66]. Clariana et al [67] found this technique better than CG-FID in a study performed with pork meat. Due to the necessity of a derivatization process and the impossibility of analysing thermolabile molecules, some liquid chromatography methods have been recently developed [68][69][70].…”

Dietary cholesterol oxidation products: Perspectives linking food processing and storage with health implications

“…After the proper pretreatment of food samples, the COPs of interest can be analyzed using instruments. The instrumental techniques mainly involve thin‐layer chromatography (TLC), HPLC equipped with ultraviolet‐visible spectroscopy detector (UV‐Vis) or diode array detector (DAD), HPLC‐MS/MS, GC equipped with flame ionization detector (FID), GC‐MS, and GC‐MS/MS (Baggio & Bragagnolo, 2006; Baggio et al., 2005; Clariana et al., 2011; Janoszka, 2010; Kamgang Nzekoue et al., 2020; Leal‐Castaneda et al., 2017). TLC is a widely used, fast, and relatively economical method for separating mixtures.…”

“…They are used in combination to silylate COP to trimethylsilyl ether. In previous studies, pyridine/BSTFA/TMCS, pyridine/HMDS/TMCS, and pyridine/BSTFA/TMCS/TMSI were used for derivatization of COPs from milk, dry‐cured shoulder, and ham, respectively (Calderón‐Santiago et al., 2012; Chiu et al., 2018; Clariana et al., 2011).…”

Novel approach to fast determination of cholesterol oxidation products in Cypriot foodstuffs using ultra-performance liquid chromatography-tandem mass spectrometry

“…Cholesterol oxidation products, commonly known as cholesterol oxidation products (COPs), comprise a variety of compounds deriving from oxidation of cholesterol. In the last decades, COPs have been one of the most intense topics in food science due to their link to a series of biological effect . These compounds have been well documented for being potentially cytotoxic, mutagenic, carcinogenic, and they have been associated with the promotion of atherosclerosis .…”

“…A study by Clariana M. et al. reported the determination of COPs in dry‐cured shoulder, a traditional Spanish meat that is similar to Cypriot cold meats . During the curing process, an abusive condition, such as extensive salting, dehydration, and exposure to air, occurred.…”