Valerian Tablets
DEFINITION
Valerian Tablets contain Powdered Valerian Extract. Tablets contain NLT 90.0% and NMT 120.0% of the labeled amount of Powdered Valerian Extract, calculated as valerenic acid (C15H22O2).
IDENTIFICATION
• A. Thin-Layer Chromatographic Identification Test 
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Standard solution:
0.5 mg/mL each of USP Fluorescein RS and USP Valerenic Acid RS in methanol
Sample solution:
Transfer an equivalent to 100 mg of Powdered Valerian Extract from finely powdered Tablets (NLT 10) 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 in a water bath at 40
for 10 min, 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.
for 10 min, 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.
Adsorbent:
0.5-mm layer of chromatographic silica gel mixture
Application volume
Standard solution:
10 µL
Sample solution:
20 µL, in a 2-cm band
Developing solvent system:
Solvent hexane, ethyl acetate, and glacial acetic acid (65:35:0.5)
Spray reagent:
Mix 0.5 mL of anisaldehyde with 10 mL of glacial acetic acid, 85 mL of methanol, and 5 mL of sulfuric acid, added in the sequence specified.
Analysis
Samples:
Standard solution and Sample solution
Spray the plate with Spray reagent. Heat the plate in an oven at 105 for 10 min, and examine the plate under white light.
for 10 min, and examine the plate under white light.
Acceptance criteria:
The Standard solution chromatogram shows a violet zone due to valerenic acid at an RF value of 0.4, and a yellow zone due to fluorescein at an RF value of 0.1. The Sample solution chromatogram shows a violet zone due to valerenic acid at an RF value of 0.4, and a blue-violet zone due to hydroxyvalerenic acid at an RF value of 0.12, just above the yellow zone in the Standard solution. The Sample solution chromatogram may show other colored zones at RF values lower than those of valerenic acid.
• B.
The retention time of the valerenic acid peak of the Sample solution corresponds to that of the Standard solution, as obtained in the test for Content of Valerenic Acid.
STRENGTH
• Content of Valerenic Acid
Mobile phase:
Methanol and water (77:27). Add 0.5 mL of phosphoric acid to each 100 mL of the mixture.
System suitability solution:
24 µg/mL of USP Valerenic Acid RS in methanol
Standard solution:
3.5 µg/mL of USP Valerenic Acid RS in methanol
Sample solution:
Weigh NLT 20 Tablets, and pulverize with a mortar and pestle. Transfer a portion of the powder, nominally equivalent to 0.09 mg of valerenic acid, to a suitable flask. Add 25.0 mL of methanol, shake to disperse the powder, sonicate for 10 min, and centrifuge. Use the clear supernatant.
Chromatographic system
Mode:
LC
Detector:
UV 225 nm
Column:
4.6-mm × 25-cm; packing L1
Column temperature:
30
Flow rate:
1.5 mL/min
Injection size:
20 µL
System suitability
Sample:
System suitability solution
Suitability requirements
Capacity factor, k¢:
NLT 5, determined from valerenic acid
Tailing factor:
NMT 2.0 for valerenic acid
Relative standard deviation:
NMT 2.0% for valerenic acid
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of Extract as valerenic acid in the portion of Tablets taken:
Result = (rU/rS) × (CS × V/W) × (100/LE) × (AW × 100/L)
| rU | = | = peak response from the Sample solution |
| rS | = | = peak response from the Standard solution |
| CS | = | = concentration of USP Valerenic Acid RS in the Standard solution (mg/mL) |
| V | = | = volume of the Sample solution (mL) |
| W | = | = weight of the sample of powdered Tablets used to prepare the Sample solution (mg) |
| AW | = | = average weight of the Tablets (mg/Tablet) |
| LE | = | = labeled amount of valerenic acid in 100 mg of the Extract used to prepare the Tablets (mg) |
| L | = | = labeled amount of Extract per Tablet (mg/Tablet) |
Acceptance criteria:
90.0%–120.0%
PERFORMANCE TESTS
• Disintegration and Dissolution of Dietary Supplements 2040:
Meet the requirements for Disintegration
2040:
Meet the requirements for Disintegration
• Weight Variation of Dietary Supplements 2091:
Meet the requirements
2091:
Meet the requirements
CONTAMINANTS
• Microbial Enumeration Tests 2021:
The total aerobic microbial count does not exceed 10,000 cfu/g, and the total combined molds and yeasts count does not exceed 1000 cfu/g.
2021:
The total aerobic microbial count does not exceed 10,000 cfu/g, and the total combined molds and yeasts count does not exceed 1000 cfu/g.
• Microbial Procedures for Absence of Specified Microorganisms 2022:
Meet the requirements of the tests for absence of Salmonella species and Escherichia coli
2022:
Meet the requirements of the tests for absence of Salmonella species and Escherichia coli
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in tight, light-resistant containers, and store at room temperature.
• 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.
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Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Maged H. Sharaf, Ph.D.
Principal Scientific Liaison 1-301-816-8318 |
(DS2010) Monographs - Dietary Supplements |
| 2021 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
| 2022 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 1466
Pharmacopeial Forum: Volume No. 36(1) Page 169