Powdered Valerian
DEFINITION
Powdered Valerian is Valerian reduced to a fine or a very fine powder. It contains no calcium oxalate crystals and no foreign starch granules. It contains NLT 0.3% of volatile oil and NLT 0.04% of valerenic acid (C15H22O2).
IDENTIFICATION
• A. Color Reaction
Sample solution:
0.2 g of Powdered Valerian in 5 mL of methylene chloride. Shake several times, and allow to stand for 5 min. Filter, wash the filter with 2 mL of methylene chloride, and combine the filtrate and washings in one container. Heat the combined filtrate and washings on a water bath for the minimum time required to evaporate the solvent, and dissolve the residue in 0.2 mL of methylene chloride.
Analysis:
To 0.1 mL of the Sample solution add 3 mL of a mixture of equal volumes of glacial acetic acid and 25% hydrochloric acid, and shake several times.
Acceptance criteria:
A blue color develops within 15 min.
• B. HPLC Identification Test
Analysis:
Proceed as directed in the test for Content of Valerenic Acid.
Acceptance criteria:
The Sample solution chromatogram exhibits a peak for valerenic acid at a retention time that corresponds to that of the Standard solution.
COMPOSITION
• Content of Valerenic Acid
Mobile phase:
A (4:1) mixture of methanol and dilute phosphoric acid (1 in 200)
Standard solution:
0.05 mg/mL of USP Valerenic Acid RS in 70% alcohol
Sample solution:
To 2 g of Powdered Valerian add 40.0 mL of 70% alcohol. Shake by mechanical means for 2 h at room temperature. Centrifuge, and use the clear extract.
Chromatographic system
Mode:
LC
Detector:
UV 225 nm
Column:
4.6-mm × 25-cm; packing L1
Flow rate:
1.5 mL/min
Injection size:
20 µL
System suitability
Sample:
Standard solution
Suitability requirements
Tailing factor:
NMT 2.0 for the valerenic acid peak
Relative standard deviation:
NMT 2.0% for the valerenic acid peak
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of valerenic acid (C15H22O2) in the portion of Powdered Valerian taken:
Result = (rU/rS) × CS × (V/W) × 100
| rU | = | = peak area from the Sample solution |
| rS | = | = peak area from the Standard solution |
| CS | = | = concentration of USP Valerenic Acid RS in the Standard solution (mg/mL) |
| V | = | = volume of the Sample solution, 40 mL |
| W | = | = weight of Powdered Valerian taken to prepare the Sample solution (mg) |
Acceptance criteria:
NLT 0.04% on the dried basis
• Articles of Botanical Origin, Volatile Oil Determination 
561
561
Sample:
100 g
Acceptance criteria:
NLT 0.3%
CONTAMINANTS
• Heavy Metals 231:
50 µg/g
231:
50 µg/g
• Articles of Botanical Origin, General Method for Pesticide Residues Analysis 561:
Meets the requirements
561:
Meets the requirements
• Microbial Enumeration Tests 2021:
The total bacterial count does not exceed 105 cfu/g, the total combined molds and yeasts count does not exceed 103 cfu/g, and bile-tolerant Gram-negative bacteria does not exceed 103 cfu/g.
2021:
The total bacterial count does not exceed 105 cfu/g, the total combined molds and yeasts count does not exceed 103 cfu/g, and bile-tolerant Gram-negative bacteria does not exceed 103 cfu/g.
• Absence of Specified Microorganisms 2022:
It meets the requirements of the tests for absence of Salmonella species and Escherichia coli.
2022:
It meets the requirements of the tests for absence of Salmonella species and Escherichia coli.
SPECIFIC TESTS
• Botanic Characteristics
Microscopic:
Numerous fragments of parenchyma cells containing globules of volatile oil and starch granules; fragments of scalariform and reticulate thickened vessels and tracheids and strongly lignified narrow fibers; fragments of periderm and of piliferous layer with root hairs; numerous starch granules, rarely simple, mostly compounds of 2–6 components, spheroidal, plano-convex, 3–20, mostly from 8 to 12 µm in diameter with a central hilum, the starch granules being from 7 to 30 µm in diameter
• Extractable Matter
Sample:
2 g, carefully dried at 40
Analysis:
Mix the Sample with 20 mL of 70% alcohol, and allow to stand for 2 h, shaking frequently. Filter, evaporate 5 mL of the filtrate on a water bath to dryness, and dry the residue at 105.
.
Acceptance criteria:
NLT 20%. The weight of the dried residue is NLT 100 mg.
• Water, Method 1a 921:
NMT 5.0%
921:
NMT 5.0%
• Articles of Botanical Origin, Total Ash 561:
NMT 12.0%
561:
NMT 12.0%
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers, store at room temperature, and protect from light and moisture.
• Labeling:
The label states the Latin binomial and, following the official name, the parts of the plant from which the article was derived.
• USP Reference Standards 11
11
USP Valerenic Acid RS 
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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 1464
Pharmacopeial Forum: Volume No. 32(2) Page 395