Saw Palmetto Capsules
» Saw Palmetto Capsules contain Saw Palmetto Extract. Capsules contain not less than 22.0 percent of lauric acid and not more than 34.0 percent of the labeled amount of Saw Palmetto Extract. The ratio of the concentrations of lauric acid to caprylic acid is not less than 8.5 and not more than 17.5. The ratio of the concentrations of lauric acid to myristic acid is not less than 2.2 and not more than 2.8.
Packaging and storage Preserve in tight, light-resistant containers.
Labeling The label states the Latin binomial and, following the official name, the name of article from which the Capsules were prepared. Label it to indicate the amount of Extract in mg per Capsule.
USP Reference standards 11
USP Methyl Caprate RS.
USP Methyl Caproate RS.
USP Methyl Caprylate RS.
USP Methyl Laurate RS.
USP Methyl Linoleate RS.
USP Methyl Linolenate RS.
USP Methyl Myristate RS.
USP Methyl Oleate RS.
USP Methyl Palmitate RS.
USP Methyl Palmitoleate RS.
USP Methyl Stearate RS.
USP -Sitosterol RS.
A: The retention times of the peaks for methyl caprate, methyl caproate, methyl caprylate, methyl laurate, methyl linoleate, methyl linolenate, methyl myristate, methyl oleate, methyl palmitate, methyl palmitoleate, and methyl stearate in the chromatogram of the Test solution correspond to those in the chromatogram of the Standard solution, as obtained in the test for Content of lauric acid and the ratios of the concentrations of lauric acid to caprylic acid and lauric acid to myristic acid.
B: Presence of sterols
Derivatizing reagent, Standard solution, and Chromatographic system Proceed as directed for Content of sterols under Saw Palmetto Extract.
Test solution Take a number of Capsules, equivalent to about 10 g of extract, open the Capsules using a suitable cutting instrument, and transfer the shells and contents to a suitable container. Transfer about 5 g, accurately weighed, to a 250-mL round-bottom flask, and evaporate in vacuum at a temperature not exceeding 50. Add 50 mL of a solution prepared by dissolving 130 g of potassium hydroxide in 200 mL of water and diluting with methanol to 1000 mL. Attach a condenser, and reflux in a bath at 100 until a clear solution is obtained. Reflux for an additional 10 minutes, and cool by adding 50 mL of water through the condenser. Quantitatively transfer to a separation funnel, rinsing the flask with a total of 50 mL of water in small portions. Extract with 80 mL of ether, shaking for 30 seconds, and repeat twice. [noteIf an emulsion forms, it can be eliminated by adding small quantities of methanol.] Transfer the combined ether layers to a separation funnel, and wash with successive portions of 50 mL of water until a neutral washing is obtained. [noteIf an emulsion forms, it can be eliminated by adding small quantities of methanol.] Pass the ether extract through filter paper containing anhydrous sodium sulfate, wash the filter with 30 mL of ether, and evaporate to dryness in vacuum. Dissolve the residue in 2.0 mL of chloroform.
Apply separately 200 µL of this solution and 20 µL of a solution of -cholestanol in chloroform (1 in 100) to a thin-layer chromatographic plate coated with 0.25-mm silica gel having an application zone that was previously dipped under 3 cm of a solution prepared by dissolving 13 g of potassium hydroxide in 20 mL of water and diluted to 1000 mL with methanol. [noteAllow the plate to dry, and heat it to 100 for 1 hour before use. The plate can be stored in a desiccator containing calcium chloride until the time of use.] Develop with a solvent consisting of a mixture of hexanes and ether (7:3) until the solvent front has moved 17 to 19 cm. Keep the chamber temperature between 15 and 20. Dry the plate in a current of warm air, then spray with an alkaline solution of 2,7-dichlorofluorescein in alcohol (0.2 in 100). Observe the plate under 366-nm wavelength light and identify the bands corresponding to the sterols by referring to the -cholestanol spot. Scrape off these bands and transfer them to a test tube. Add 10 mL of warm chloroform, and shake for 2 minutes with the aid of several glass beads. Filter the chloroform solution, wash the filter with chloroform, and evaporate the combined filtrate and washings to dryness in vacuum. Dissolve the residue with some drops of anhydrous acetone and evaporate in vacuum. Dry the residue in an oven at 105 for 15 minutes. Dissolve the residue in 0.2 mL of Derivatizing reagent, and allow to stand for not less than 15 minutes at room temperature.
Procedure Proceed as directed for Content of sterols under Saw Palmetto Extract. The chromatogram of the Test solution exhibits peaks for campesterol, -sitosterol, and stigmasterol, identified by their retention times relative to the -sitosterol peak in the chromatogram of the Standard solution.
Microbial enumeration 2021 Capsules meet the requirements of the tests for absence of Salmonella species, Escherichia coli, and Staphylococcus aureus. The total bacterial count does not exceed 10,000 cfu per g, the total combined molds and yeasts count does not exceed 1000 cfu per g, the coliform count does not exceed 100 cfu per g, and the count for enterobacteria does not exceed 100 cfu per g.
Medium: simulated gastric fluid TS; 500 mL.
Apparatus 2: 50 rpm (see Apparatus under Disintegration and Dissolution of Dietary Supplements 2040).
Time: 15 minutes.
Procedure Place 1 Capsule in each vessel, and allow the Capsule to sink to the bottom of the vessel before starting rotation of the blade. Record the time it takes for each Capsule shell to rupture.
Tolerances The requirements are met if all of the Capsules rupture in not more than 15 minutes. If 1 or 2 of the Capsules rupture in more than 15 but not more than 30 minutes, repeat the test on 12 additional Capsules. Not more than 2 of the 18 Capsules tested rupture in more than 15 but not more than 30 minutes.
Weight variation 2091: meet the requirements.
Content of lauric acid and the ratios of the concentrations of lauric acid to caprylic acid and lauric acid to myristic acid
Internal standard solution, Standard solution, and Chromatographic system Proceed as directed for Content of fatty acids under Saw Palmetto.
Test solution Take a number of Capsules, equivalent to about 10 g of extract, open the Capsules using a suitable cutting instrument, and transfer the shells and contents to a suitable container. Transfer about 100 mg, accurately weighed, to a pressure-proof screw-capped vial, and add 3.0 mL of a solution of sulfuric acid in methanol (5 in 100). Heat in an oil bath at 100 for 2 hours, shaking from time to time. Allow to cool, and add 1.0 mL of Internal standard solution, 10.0 mL of water, 1 g of sodium chloride, and 5 mL of hexanes. Shake well, and allow the layers to separate completely. Use the hexanes layer. [noteStore this solution in a refrigerator until use.]
Procedure Proceed as directed for Content of fatty acids under Saw Palmetto. Identify the peaks of methyl caprate, methyl caproate, methyl caprylate, methyl laurate, methyl linoleate, methyl linolenate, methyl myristate, methyl oleate, methyl palmitate, methyl palmitoleate, and methyl stearate in the chromatogram of the Test solution. Calculate the quantity, in mg, of lauric acid, myristic acid, and caprylic acid in the portion of Capsules taken by the formula,
5C(RU / RS)(MA / ME)in which the terms are as defined therein. Using these quantities, calculate the individual ratios of the concentration of lauric acid to caprylic acid and of lauric acid to myristic acid in the portion of Capsules taken.
Auxiliary Information Please check for your question in the FAQs before contacting USP.Chromatographic Column
USP32NF27 Page 1072Pharmacopeial Forum: Volume No. 29(4) Page 1291
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.