Valerian
DEFINITION
Valerian consists of the subterranean parts of Valeriana officinalis L. (Fam. Valerianaceae) including the rhizome, roots, and stolons. It contains NLT 0.5% of volatile oil and NLT 0.05% of valerenic acid (C15H22O2), calculated on the dried basis.
IDENTIFICATION
• A. Color Reaction
Sample solution:
0.2 g of freshly 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 Valerian, reduced to a powder, 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 Valerian taken:
Result = (rU/rS) × CS × (V/W) × 100
Acceptance criteria:
NLT 0.05% on the dried basis
• Articles of Botanical Origin, Volatile Oil Determination 561
Sample:
100 g, freshly and coarsely comminuted
Acceptance criteria:
NLT 0.5% on the dried basis
CONTAMINANTS
• Articles of Botanical Origin, General Method for Pesticide Residues Analysis 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.
• Absence of Specified Microorganisms 2022:
It meets the requirements of the tests for absence of Salmonella species and Escherichia coli.
SPECIFIC TESTS
• Botanic Characteristics
Macroscopic:
Rhizome erect, entire or usually cut longitudinally, up to 5 cm in length and up to 3 cm in diameter, yellowish gray to pale grayish brown, base elongated or compressed, covered by and merging with numerous roots; apex usually bearing a cup-shaped scar from aerial parts, stem bases rarely present; in longitudinal section, pith exhibiting a central cavity traversed by septa. Roots numerous, slender, almost cylindrical, and of the same color as the rhizome, about 10 cm in length and up to 3 mm in diameter; a few filiform, fragile secondary roots; fracture short. Stolon pale yellowish gray, showing prominent nodes separated by longitudinally striated internodes each from 2 to 5 cm in length; fracture fibrous.
Microscopic:
Root, with piliferous layer, of papillosed cells, some being developed into root hairs; exodermis, or a single layer of quadrangular to polygonal cells with suberized walls and containing globules of volatile oil; outer cortex of two to four layers of resin-containing cells with thin or collenchymatous, sometimes suberized walls; inner cortex of numerous layers of polygonal to rounded cells filled with starch. Starch granules simple or compound; simple granules rounded, from 5 to 15 µm in diameter, sometimes showing a cleft or stellate hilum; compound granules with 26 components, up to 20 µm in diameter. Endodermis consisting of a single layer of suberized, tangentially elongated cells, pericycle continuous, starch-filled; parenchyma surrounding the phloem zone; cambium frequently indistinct; vascular bundles forming an interrupted ring surrounding the starch-filled cells. Rhizome in transverse section, different from the root, its structure being complicated by the presence of numerous vascular bundles from root and stolon; epidermis and exodermis partially replaced by poorly developed periderm; central pith wide, including cavities of various sizes, the larger ones being separated by plates of partially sclerified tissue.
• Extractable Matter
Sample:
2 g, carefully dried at 40 and coarsely powdered
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.
• Articles of Botanical Origin, Water Content 561:
NMT 12.0%
• Articles of Botanical Origin, Total Ash 561:
NMT 12.0%
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in tight 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 contained in the article.
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 1463
Pharmacopeial Forum: Volume No. 32(2) Page 394
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