Determination of Campesterol, Stigmasterol, and Beta-Sitosterol in Saw Palmetto Raw Materials and Dietary Supplements by Gas Chromatography: Collaborative Study

Sorenson, Wendy R; Sullivan, Darryl; Baugh, Steve; Collison, Mark W.; Das, Rashmita; Erickson, Aron; Harmon, Tiffany; Heathman, S; Ji, David; Khandelwal, B; Kohn, Andrew; Morris, Stephen; Norden, Denise; Tian, Peng; Post, Brett E; Powers, Edmund M.; Reif, K.; Schulzki, G.; Shevchuk, C; Solyom, Aniko M

doi:10.1093/jaoac/90.3.670

Cited by 27 publications

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“…Although suggested by Fenton (1992) as a common practice, the addition of 5α-cholestane in the beginning of sample preparation was found to be unnecessary (Dinh 2010). Sorenson and Sullivan (2007) came to the same conclusion in their collaborative study on GC determination of phytosterols.…”

Section: Internal Standards For Cholesterol Quantificationmentioning

confidence: 62%

Cholesterol Content and Methods for Cholesterol Determination in Meat and Poultry

Dinh

Thompson

Galyean

et al. 2011

Comp Rev Food Sci Food Safe

104

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Available data for cholesterol content of beef, pork, poultry, and processed meat products were reported. Although the cholesterol concentration in meat and poultry can be influenced by various factors, effects of animal species, muscle fiber type, and muscle fat content are focused on in this review. Oxidative red muscles tend to have greater total lipid and cholesterol contents, although differences in the same types of muscles or cuts have been reported. Moreover, contradictory results among various studies suggest that unless there are pronounced changes in muscle structure and composition, cholesterol content is unlikely to be affected. Second, multiple issues in cholesterol analysis, including sample preparation, detection, and quantification, were evaluated. Cholesterol content of meat and poultry has been determined mostly by colorimetry and chromatography, although the latter has become predominant because of technological advances and method performance. Direct saponification has been the preferred method for hydrolyzing samples because of cost‐ and time‐effectiveness. The extraction solvent varies, but toluene seems to provide sufficient recovery in a single extraction, although the possible formation of an emulsion associated with using toluene requires experience in postsaponification manipulation. The most commonly used internal standard is 5α‐cholestane, although its behavior is not identical to that of cholesterol. Cholesterol can be analyzed routinely by gas chromatography (GC)‐flame ionization detector without derivatization; however, other methods, especially high‐performance liquid chromatography (HPLC) coupled with different detectors, can also be used. For research purposes, HPLC‐ultraviolet/Visible/photodiode array detector with nondestructiveness is preferred, especially when cholesterol must be separated from other coexisting compounds such as tocopherols. More advanced methods, such as GC/HPLC‐isotope dilution/mass spectrometry, are primarily used for quality control purposes.

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Section: Internal Standards For Cholesterol Quantificationmentioning

confidence: 62%

Cholesterol Content and Methods for Cholesterol Determination in Meat and Poultry

Dinh

Thompson

Galyean

et al. 2011

Comp Rev Food Sci Food Safe

104

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“…Phytosterol content in Echium oils was achieved through oil saponification at 80 C for 80 min under reflux using a 50% KOH aqueous solution and further extraction of the unsaponifiable fraction with toluene, sterol derivatization to trimethylsilyl ethers using hexamethyldisilane and trimethylchlorosilane as derivatizing reagents, and GC-FID analysis according to a modified AOAC official method 994.10 as described in (Sorenson and Sullivan, 2006). An amount of 0.45 g oil was used for phytosterol analysis.…”

Section: Analysis Of Phytosterolsmentioning

confidence: 99%

Fatty Acid Profile and Bioactive Compound Extraction in Purple Viper's Bugloss Seed Oil Extracted with Green Solvents

Rincón‐Cervera

Galleguillos‐Fernández

González‐Barriga

et al. 2020

J Americ Oil Chem Soc

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Oil extraction from seeds of purple viper's bugloss (Echium plantagineum) was carried out using different solvents (chloroform:methanol, n‐hexane, ethanol, 2‐propanol and ethyl acetate) at room temperature and also using Randall extraction. Extraction yields were calculated and oils were analyzed in terms of fatty acid profiles and distribution among lipid classes, total polyphenol content, oxygen radical absorbance capacity (ORAC) and phytosterol content. No considerable differences were found on fatty acid profiles and distribution in oils regardless of the solvent and temperature used for the extraction. However, ethanol combined with Randall extraction (85 °C for 1 hour) offered the best results in terms of total polyphenol content (20.9 mg GAE/100 g oil), ORAC (468.0 μmol TE/100 g oil), and phytosterol amount (437.2 mg identified phytosterols/100 g oil) among all assayed extraction methods. A higher extraction temperature led to significantly higher concentrations of bioactive compounds and ORAC values in the oil when ethanol or 2‐propanol were used as extracting solvent, but that was not the case using n‐hexane except for the concentrations of β‐sitosterol and stigmasterol, which were significantly higher using Randall extraction than room temperature extraction with n‐hexane. Ethanol is classified as a “green solvent,” and it could be considered a suitable option to produce oil from E. plantagineum seeds with a higher antioxidant capacity and bioactive compound concentration than the current commercial oil, which is usually extracted with n‐hexane.

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“…The objective of this international, multilaboratory collaborative study was to validate a method for the determination of plant sterols and stanols in foods and dietary supplements containing added phytosterols and in the phytosterol food additive concentrates used to prepare such products. When compared with other collaboratively studied methods for phytosterols (Laakso, ; Sorenson & Sullivan, ), the chromatographic resolution of the five major phytosterols, including the separation of sitostanol and Δ5‐avenasterol, is unique to this method. Such a separation is required to support FDA's health claim regulation (Department of Health and Human Services, Food and Drug Administration, ).…”

Section: Resultsmentioning

confidence: 99%

“…Phytosterols are routinely analyzed by using gas chromatography with flame ionization detection (GC‐FID) after derivatization to trimethylsilyl (TMS) ethers. In the 2010 Proposed Rule (Department of Health and Human Services, Food and Drug Administration, ), FDA considered replacing the Unilever and McNeil methods of analysis (Department of Health and Human Services, Food and Drug Administration, ), which were specified for plant sterol and stanol esters, respectively, with Official Method 994.10 (AOAC INTERNATIONAL, ) of the AOAC INTERNATIONAL as modified by Sorenson and Sullivan (, ). However, this modified method was validated only for campesterol, stigmasterol, and β‐sitosterol at concentrations of ≤0.5 g 100 g −1 in saw palmetto raw materials, extracts, and dietary supplements.…”

Section: Introductionmentioning

confidence: 99%

Sterols and Stanols in Foods and Dietary Supplements Containing Added Phytosterols: A Collaborative Study

Srigley

Hansen

Smith

et al. 2018

J Americ Oil Chem Soc

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An international, multilaboratory collaborative study was carried out to evaluate the performance of Official Method Ce 12-16 of the American Oil Chemists' Society (AOCS) for the determination of plant sterols and stanols, collectively referred to as phytosterols, in foods and dietary supplements containing added phytosterols and in the phytosterol food additive concentrates used to prepare such products. AOCS Official Method Ce 12-16 involves the extraction of free sterols/stanols and saponified steryl/stanol esters followed by the gas chromatographic separation and flame ionization detection of phytosterol trimethylsilyl ether derivatives. A total of 14 laboratories from six countries successfully completed the analysis of collaborative samples of foods (e.g., baked goods, beverages, margarines; n = 9), dietary supplements (n = 5), and phytosterol concentrates (n = 4). Study results for the contents of total phytosterols (weight/weight) were 0.19-8.4% for foods, 8.7-49% for dietary supplements, and 57-97% for concentrates. AOCS Official Method Ce 12-16 showed acceptable performance for total and individual phytosterols, indicating that this method was suitable for the determination of added phytosterols in a wide variety of market products and concentrates. AOCS Official Method Ce 12-16 is appropriate for the determination of the five major phytosterols (i.e., campesterol, stigmasterol, β-sitosterol, campestanol, and sitostanol) that are the subject of the United States Food and Drug Administration's health claim for phytosterols and the reduced risk of coronary heart disease.

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Determination of Campesterol, Stigmasterol, and Beta-Sitosterol in Saw Palmetto Raw Materials and Dietary Supplements by Gas Chromatography: Collaborative Study

Cited by 27 publications

References 0 publications

Cholesterol Content and Methods for Cholesterol Determination in Meat and Poultry

Cholesterol Content and Methods for Cholesterol Determination in Meat and Poultry

Fatty Acid Profile and Bioactive Compound Extraction in Purple Viper's Bugloss Seed Oil Extracted with Green Solvents

Sterols and Stanols in Foods and Dietary Supplements Containing Added Phytosterols: A Collaborative Study

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