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).
• 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.
• 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.
Detector: UV 225 nm
Column: 4.6-mm × 25-cm; packing L1
Flow rate: 1.5 mL/min
Injection size: 20 µL
Sample: Standard solution
Tailing factor: NMT 2.0 for the valerenic acid peak
Relative standard deviation: NMT 2.0% for the valerenic acid peak
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
Acceptance criteria: NLT 0.04% on the dried basis
• Articles of Botanical Origin, Volatile Oil Determination 561
Sample: 100 g
Acceptance criteria: NLT 0.3%
• Heavy Metals 231: 50 µg/g
• 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.
• 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 26 components, spheroidal, plano-convex, 320, 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%
• Articles of Botanical Origin, Total Ash 561: NMT 12.0%
• 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
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USP35NF30 Page 1464Pharmacopeial Forum: Volume No. 32(2) Page 395