Packaging and storage—
Preserve in tight, light-resistant containers.
Labeling—
The label states the Latin binomial and, following the official name, the article from which the Tablets were prepared. The label also indicates the quantity, in mg, of Powdered Valerian Extract per Tablet and the content, in mg, of valerenic acid per 100 mg of Powdered Valerian Extract.
Identification—
A:
Thin-Layer Chromatographic Identification Test 
201
—
Test solution—
Weigh and finely powder not fewer than 10 Tablets. Transfer a portion of the powder, equivalent to about 100 mg of Powdered Valerian Extract, to a suitable flask. Add 5 mL of water and 3 mL of a 10% aqueous solution of potassium hydroxide, extract this mixture with two 5-mL portions of methylene chloride, and discard the organic phase. Heat the aqueous phase on a water bath at 40
for 10 minutes, cool, acidify with 7% hydrochloric acid, and extract this solution with two 5-mL portions of methylene chloride. Dry the organic phase over anhydrous sodium sulfate, filter, evaporate the filtrate to dryness, and dissolve the residue in 1.0 mL of methylene chloride. Apply 20 µL to the plate in a 2-cm band.
B:
The retention time of valerenic acid in the chromatogram of the Test solution corresponds to that in the chromatogram of the Standard solution, as obtained in the test for Content of valerenic acid.
Microbial enumeration 2021—
It meets the requirements of the tests for absence of
Salmonella species and
Escherichia coli. The total aerobic microbial count does not exceed 10,000 cfu per g, and the total combined molds and yeasts count does not exceed 1000 cfu per g.
Content of valerenic acid—
Mobile phase, Standard preparation, and Chromatographic system—
Proceed as directed in the test for
Content of valerenic acid under
Powdered Valerian Extract. To evaluate the system suitability requirements, use the
Standard preparation.
Standard solution—
Dissolve an accurately weighed quantity of
USP Valerenic Acid RS in methanol, and dilute quantitatively, and stepwise if necessary, with methanol to obtain a solution having a known concentration of about 3.5 µg per mL.
Test solution—
Weigh accurately not fewer than 20 Tablets, and pulverize with a mortar and pestle. Transfer an accurately weighed portion of the powder, equivalent to about 0.09 mg of valerenic acid, to a suitable flask. Add 25.0 mL of methanol, shake to disperse the powder, sonicate for 10 minutes, and centrifuge. Use the clear supernatant.
Procedure—
Separately inject equal volumes (about 20 µL) of the
Standard solution and the
Test solution into the chromatograph, record the chromatograms, and measure the responses for the valerenic acid peaks. Calculate the quantity, in mg, of valerenic acid (C
15H
22O
2) in the portion of Tablets taken by the formula:
25C(rU / rS),
in which
C is the concentration, in mg per mL, of
USP Valerenic Acid RS in the
Standard solution; and
rU and
rS are the peak responses obtained from the
Test solution and the
Standard solution, respectively.
Auxiliary Information—
Staff Liaison :
Maged H. Sharaf, Ph.D., Senior Scientist
Expert Committee : (DSB05) Dietary Supplements - Botanicals
USP29–NF24 Page 2386
Pharmacopeial Forum : Volume No. 27(1) Page 1827
Phone Number : 1-301-816-8318
