Development of a fast sample treatment for the analysis of free and bonded sterols in human serum by <scp>LC</scp>‐<scp>MS</scp>

Mendiara, I.; Domeño, Celia; Nerı́n, Cristina

doi:10.1002/jssc.201200519

Cited by 19 publications

(23 citation statements)

References 37 publications

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“…Mendiara, et al . [29] used LC-MS with APCI but no MS-MS with a 20-min cycle time between analyses, and Zarrouk, et al . [19] used APCI LC-MS-MS with a 65-min separation.…”

Section: Resultsmentioning

confidence: 99%

Quantitative Analysis of Phytosterols in Edible Oils Using APCI Liquid Chromatography–Tandem Mass Spectrometry

Hurst

et al. 2013

Lipids

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Previous methods for the quantitative analysis of phytosterols have usually used GC-MS and require elaborate sample preparation including chemical derivatization. Other common methods such as HPLC with absorbance detection do not provide information regarding the identity of the analytes. To address the need for an assay that utilizes mass selectivity while avoiding derivatization, a quantitative method based on LC-tandem mass spectrometry (LC-MS-MS) was developed and validated for the measurement of six abundant dietary phytosterols and structurally related triterpene alcohols including brassicasterol, campesterol, cycloartenol, β-sitosterol, stigmasterol, and lupeol in edible oils. Samples were saponified, extracted with hexane and then analyzed using reversed phase HPLC with positive ion atmospheric pressure chemical ionization tandem mass spectrometry and selected reaction monitoring. The utility of the LC-MS-MS method was demonstrated by analyzing 14 edible oils. All six compounds were present in at least some of the edible oils. The most abundant phytosterol in all samples was β-sitosterol, which was highest in corn oil at 4.35 ± 0.03 mg/g, followed by campesterol in canola oil at 1.84 ± 0.01 mg/g. The new LC-MS-MS method for the quantitative analysis of phytosterols provides a combination of speed, selectivity and sensitivity that exceed those of previous assays.

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“…Mendiara, et al . [29] used LC-MS with APCI but no MS-MS with a 20-min cycle time between analyses, and Zarrouk, et al . [19] used APCI LC-MS-MS with a 65-min separation.…”

Section: Resultsmentioning

confidence: 99%

Quantitative Analysis of Phytosterols in Edible Oils Using APCI Liquid Chromatography–Tandem Mass Spectrometry

Hurst

et al. 2013

Lipids

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“…Several publications dealing with online systems are focused on determining drugs in plasma or urine; but scarce literature has been found related to the determination of endogenous metabolites [18,19]. A previous work of the authors aimed at the reduction of the sample processing time for determining free and bonded sterols in human serum [20,21] [22]. To the best of our knowledge, there is not such a system to determine sterols in human serum, so the present contribution aims at the routine analysis of sterols in a faster way by using an online system.…”

Section: Introductionmentioning

confidence: 98%

Online solid-phase extraction–liquid chromatography–mass spectrometry to determine free sterols in human serum

Mendiara

Bentayeb

Nerı́n

et al. 2015

Talanta

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An automated method for analyzing free non-cholesterol sterols in human serum using online solid phase extraction-liquid chromatography-mass spectrometry is proposed herein. The method allows the determination of three phytosterols (sitosterol, stigmasterol and campesterol) and two cholesterol precursors (desmosterol and lanosterol). The analysis of sterols in human serum is critical in the study of cholesterol-related disorders, such as inherited familial hypercholesterolemias. Special effort was made to isolate the analytes from the serum lipoproteins, their natural conveyance through the bloodstream. The sample treatment consisted of a Bligh-Dyer extraction followed by dilution of the extract. This treatment allowed the sample to be injected into the online system and ensured the correct detection of the analytes, while avoiding the matrix effects commonly related to serum samples. The analytical performance showed linear ranges that covered two orders of magnitude, with correlation coefficients above 0.99. Limits of detection and quantification ranged from 0.2 ng/mL to 13 ng/mL and from 1.0 ng/mL to 43 ng/mL, respectively. Recovery when spiking serum with a half or a tenth of the average concentration reported in human serum ranged from 99% to 111% and from 102% to 120%, respectively. Intra-day precision and inter-day precision were below 20%.

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“…Cholesterol, whose metabolism is regulated, plays an essential role in living beings [14]. Recent epidemiological…”

Section: Introductionmentioning

confidence: 99%

Determination of neuroprotective oxysterols in Calculus bovis, human gallstones, and traditional Chinese medicine preparations by liquid chromatography with mass spectrometry

Wang

Jiang

Huang

et al. 2015

J of Separation Science

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So far, the components responsible for the neuroprotective effects of Calculus bovis are unclear. Cholesterol, one of the major components in Calculus bovis, is easily oxidized into oxysterols, which possess direct or indirect neuroprotective effects proved by our and others' previous studies. Therefore, a liquid chromatography with mass spectrometry method coupled with ultrasonic extraction and solid-phase extraction was developed for the determination of neuroprotective oxysterols in Calculus bovis, human gallstones, and traditional Chinese medicine preparations. Chromatographic separation was achieved on a C18 column with isocratic elution at a flow rate of 1 mL/min. The established method showed good linearity (R(2) > 0.998), sensitivity with low limits of detection (0.06-0.39 μg/g), acceptable precisions (relative standard deviations ≤ 7.4%), stability (relative standard deviations ≤ 5.9%), and satisfactory accuracy (92.4-102.9%) for all analytes identified by different retention times, which could be applied for the determination of oxysterols. Five kinds of oxysterols proved to function as neuroprotectants were detected at different concentrations. Among them, 7β-hydroxycholesterol and cholestane-3β,5α,6β-triol were rather abundant in the samples. It could be concluded that the potential neuroprotective components in Calculus bovis may be these oxysterols.

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Development of a fast sample treatment for the analysis of free and bonded sterols in human serum by LC‐MS

Cited by 19 publications

References 37 publications

Quantitative Analysis of Phytosterols in Edible Oils Using APCI Liquid Chromatography–Tandem Mass Spectrometry

Quantitative Analysis of Phytosterols in Edible Oils Using APCI Liquid Chromatography–Tandem Mass Spectrometry

Online solid-phase extraction–liquid chromatography–mass spectrometry to determine free sterols in human serum

Determination of neuroprotective oxysterols in Calculus bovis, human gallstones, and traditional Chinese medicine preparations by liquid chromatography with mass spectrometry

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