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# Fractional factorial design-based optimisation and application of an extraction and UPLC-MS/MS detection method for the quantification of phytosterols in food, feed and beverages low in phytosterols

Anneleen Decloedt (UGent) , Anita Van Landschoot (UGent) and Lynn Vanhaecke (UGent)
(2016) 408(27). p.7731-7744
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Abstract
Phytosterols are ubiquitous in plants, as they play an important role in cell membrane stability and as signal transducers. Over the last few decades, scientific interest in phytosterols has significantly increased. Most of the interest has focused on the cholesterol-lowering properties of phytosterols, but they may also interfere with endogenous steroid hormone synthesis. Despite this dual interest in phytosterols, accurate and fully validated methods for the quantification of phytosterols in food and feed samples are scarce. During this study an extraction and detection method for the main free phytosterols (β-sitosterol, campesterol, stigmasterol and brassicasterol) was optimised using a fractional factorial design. Detection was carried out on a UPLC-MS/MS triple stage quadrupole apparatus. The extraction and UPLC-MS/MS detection method was fully validated according to EU Council Decision 2002/657 guidelines and Association of Analytical Chemists (AOAC) MS criteria, reaching all evaluated performance parameter requirements. The individual recoveries ranged between 95 and 104 %. Good results for repeatability and intralaboratory reproducibility (RSD %) were observed (<10 %). Excellent linearity was proven on the basis of determination coefficient (R 2 > 0.99) and lack-of-fit test (F test, alpha = 0.05). The limits of detection (LODs) and lower limits of quantification (LLOQs) in grain matrices were as low as 0.01-0.03 mg per 100 g and 0.02-0.10 mg per 100 g. This method allowed quantification of all main, free phytosterols in different grains (oats, barley, corn, malt) and it was shown that the method can be used for other solid food and feed samples as well, including new matrices such as straw, hay, mustard seeds, grass and yellow peas. Additionally, the method was shown to perform well in liquid samples low in phytosterols such as concentrate-based juices, soft drinks and beers (<5 μg per 100 mL). Graphical Abstract An extraction and detection method for the main free phytosterols (β-sitosterol, campesterol, stigmasterol and brassicasterol) was optimised using a fractional factorial design. Detection was carried out on a UPLC-MS/MS triple stage quadrupole apparatus. The extraction and UPLC-MS/MS detection method was fully validated according to EU Council Decision 2002/657 guidelines and Association of Analytical Chemists (AOAC) MS criteria and applied on different matrices including feed and beverages.
Keywords
Ultra high-performance liquid chromatography, Extraction, Tandem mass spectrometry, Foods/beverages, Phytosterols, Bioanalytical methods, PRESSURE CHEMICAL-IONIZATION, ANABOLIC-ANDROGENIC STEROIDS, LIQUID-CHROMATOGRAPHY, PLANT STEROLS, MASS-SPECTROMETRY, CHOLESTEROL-METABOLISM, QUANTITATIVE-ANALYSIS, DIETARY PHYTOSTEROLS, BETA-SITOSTEROL, SAW PALMETTO

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## Citation

Chicago
Decloedt, Anneleen, Anita Van Landschoot, and Lynn Vanhaecke. 2016. “Fractional Factorial Design-based Optimisation and Application of an Extraction and UPLC-MS/MS Detection Method for the Quantification of Phytosterols in Food, Feed and Beverages Low in Phytosterols.” Analytical and Bioanalytical Chemistry 408 (27): 7731–7744.
APA
Decloedt, Anneleen, Van Landschoot, A., & Vanhaecke, L. (2016). Fractional factorial design-based optimisation and application of an extraction and UPLC-MS/MS detection method for the quantification of phytosterols in food, feed and beverages low in phytosterols. ANALYTICAL AND BIOANALYTICAL CHEMISTRY, 408(27), 7731–7744.
Vancouver
1.
Decloedt A, Van Landschoot A, Vanhaecke L. Fractional factorial design-based optimisation and application of an extraction and UPLC-MS/MS detection method for the quantification of phytosterols in food, feed and beverages low in phytosterols. ANALYTICAL AND BIOANALYTICAL CHEMISTRY. 2016;408(27):7731–44.
MLA
Decloedt, Anneleen, Anita Van Landschoot, and Lynn Vanhaecke. “Fractional Factorial Design-based Optimisation and Application of an Extraction and UPLC-MS/MS Detection Method for the Quantification of Phytosterols in Food, Feed and Beverages Low in Phytosterols.” ANALYTICAL AND BIOANALYTICAL CHEMISTRY 408.27 (2016): 7731–7744. Print.
@article{8083138,
abstract     = {Phytosterols are ubiquitous in plants, as they play an important role in cell membrane stability and as signal transducers. Over the last few decades, scientific interest in phytosterols has significantly increased. Most of the interest has focused on the cholesterol-lowering properties of phytosterols, but they may also interfere with endogenous steroid hormone synthesis. Despite this dual interest in phytosterols, accurate and fully validated methods for the quantification of phytosterols in food and feed samples are scarce. During this study an extraction and detection method for the main free phytosterols (\ensuremath{\beta}-sitosterol, campesterol, stigmasterol and brassicasterol) was optimised using a fractional factorial design. Detection was carried out on a UPLC-MS/MS triple stage quadrupole apparatus. The extraction and UPLC-MS/MS detection method was fully validated according to EU Council Decision 2002/657 guidelines and Association of Analytical Chemists (AOAC) MS criteria, reaching all evaluated performance parameter requirements. The individual recoveries ranged between 95 and 104 \%. Good results for repeatability and intralaboratory reproducibility (RSD \%) were observed ({\textlangle}10 \%). Excellent linearity was proven on the basis of determination coefficient (R 2\,{\textrangle}\,0.99) and lack-of-fit test (F test, alpha\,=\,0.05). The limits of detection (LODs) and lower limits of quantification (LLOQs) in grain matrices were as low as 0.01-0.03 mg per 100 g and 0.02-0.10 mg per 100 g. This method allowed quantification of all main, free phytosterols in different grains (oats, barley, corn, malt) and it was shown that the method can be used for other solid food and feed samples as well, including new matrices such as straw, hay, mustard seeds, grass and yellow peas. Additionally, the method was shown to perform well in liquid samples low in phytosterols such as concentrate-based juices, soft drinks and beers ({\textlangle}5 \ensuremath{\mu}g per 100 mL). Graphical Abstract An extraction and detection method for the main free phytosterols (\ensuremath{\beta}-sitosterol, campesterol, stigmasterol and brassicasterol) was optimised using a fractional factorial design. Detection was carried out on a UPLC-MS/MS triple stage quadrupole apparatus. The extraction and UPLC-MS/MS detection method was fully validated according to EU Council Decision 2002/657 guidelines and Association of Analytical Chemists (AOAC) MS criteria and applied on different matrices including feed and beverages.},
author       = {Decloedt, Anneleen and Van Landschoot, Anita and Vanhaecke, Lynn},
issn         = {1618-2642},
journal      = {ANALYTICAL AND BIOANALYTICAL CHEMISTRY},
language     = {eng},
number       = {27},
pages        = {7731--7744},
title        = {Fractional factorial design-based optimisation and application of an extraction and UPLC-MS/MS detection method for the quantification of phytosterols in food, feed and beverages low in phytosterols},
url          = {http://dx.doi.org/10.1007/s00216-016-9870-8},
volume       = {408},
year         = {2016},
}


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