Powdered Feverfew
DEFINITION
Powdered Feverfew is Feverfew pulverized to a fine or very fine powder.
IDENTIFICATION
• A.
The retention time of the parthenolide peak of the Sample solution corresponds to that of the Standard solution, as obtained in the test for Content of Parthenolide.
• B. Thin-Layer Chromatographic Identification Test
Standard solution:
1.0 mg/mL of USP Parthenolide RS in methanol
Sample solution:
Transfer 1.0 g of Powdered Feverfew to a suitable flask. Add 20 mL of methanol, heat the flask over a water bath at 60
for 15 min, cool, and filter. Evaporate the filtrate under reduced pressure to dryness, and dissolve the residue in 2.0 mL of methanol.
for 15 min, cool, and filter. Evaporate the filtrate under reduced pressure to dryness, and dissolve the residue in 2.0 mL of methanol.
Adsorbent:
0.5-mm layer of chromatographic silica gel, typically 20 cm long
Application volume:
20 µL
Developing solvent system:
Toluene and acetone (85:15)
Spray reagent:
0.5% solution of vanillin in a mixture of sulfuric acid and alcohol (4:1)
Analysis
Samples:
Standard solution and Sample solution
Develop the chromatograms until the solvent front has moved three-fourths of the length of the plate. Remove the plate from the chromatographic chamber, mark the solvent front, and allow it to air-dry. Spray the plate with Spray reagent. After 5 min, examine the plate in daylight.
Acceptance criteria:
A blue spot in the middle portion of the chromatogram of the Sample solution that corresponds in color and RF value to the principal spot obtained in the chromatogram of the Standard solution indicates the presence of parthenolide. The lower one-third of the chromatogram of the Sample solution may exhibit two pink spots, and the upper one-third may exhibit one pink spot.
• C. Thin-Layer Chromatographic Identification Test
Standard solution:
0.25 mg/mL of USP Rutin RS in methanol
Sample solution:
To 1 g of Powdered Feverfew, add 10 mL of methanol, and heat on a water bath at 60 for 15 min. Cool, and filter.
for 15 min. Cool, and filter.
Adsorbent:
0.25-mm layer of chromatographic silica gel, typically 20 cm long (TLC plates)
Application volume:
20 µL
Developing solvent system:
Ethyl acetate, anhydrous formic acid, glacial acetic acid, and water (10: 1.1: 1.1: 2.7)
Spray reagent A:
1% solution of 2-aminoethyl diphenylborinate in methanol
Spray reagent B:
5% (w/v) solution of polyethylene glycol 4000 in alcohol
Analysis
Samples:
Standard solution and Sample solution
Develop the chromatogram until the solvent front has moved three-fourths of the length of the plate. Remove the plate from the chromatographic chamber, and allow it to air-dry. Spray the plate with Spray reagent A followed by Spray reagent B, and examine the plate under UV light at 366 nm.
Acceptance criteria:
Relative to the RF value of the principal spot of the Standard solution, the chromatogram of the Sample solution exhibits no blue spot at RF 1.1 (distinction from Roman chamomile) but exhibits a green spot at RF 2.3 (distinction from Matricaria), and colored spots at the RF values indicated are as follows: 1.5 (yellowish orange), 1.65 (yellowish green), 2.0 (greenish blue), and 2.25 (whitish blue).
COMPOSITION
• Content of Parthenolide
Mobile phase:
Acetonitrile and water (9:11)
Standard solution:
0.04 mg/mL of USP Parthenolide RS in methanol
Sample stock solution:
Transfer about 1.0 g of the Powdered Feverfew, accurately weighed, to a suitable flask. Add 100 mL of methanol, and heat on a water bath at 60 for 10 min. Remove the flask from the water bath, cool, and filter. Rinse the flask with three 5-mL portions of methanol, and filter, adding the rinsings to the filtrate. Transfer the residue left within the filter to the same flask. Add 50 mL of methanol, and continue the rinse procedure as described above. Evaporate the combined filtrates under reduced pressure to dryness, and dissolve the residue in 20.0 mL of methanol.
for 10 min. Remove the flask from the water bath, cool, and filter. Rinse the flask with three 5-mL portions of methanol, and filter, adding the rinsings to the filtrate. Transfer the residue left within the filter to the same flask. Add 50 mL of methanol, and continue the rinse procedure as described above. Evaporate the combined filtrates under reduced pressure to dryness, and dissolve the residue in 20.0 mL of methanol.
Sample solution:
Transfer 10 mL of the Standard stock solution to a 25-mL volumetric flask, and dilute with methanol to volume.
Chromatographic system
Mode:
LC
Detector:
UV 210 nm
Column:
4.6-mm × 25-cm; packing L1
Flow rate:
2 mL/min
Injection size:
10 µL
System suitability
Sample:
Standard solution
Suitability requirements
Tailing factor:
NMT 2.0 for the parthenolide peak
Relative standard deviation:
NMT 2.0% for the parthenolide peak in repeated injections
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of parthenolide in the portion of Powdered Feverfew taken to prepare the Sample solution:
Result = (rU/rS) × CS × (V/W) × D × 100
| rU | = | = peak area of the parthenolide peak from the Sample solution |
| rS | = | = peak area of the parthenolide peak from the Standard solution |
| CS | = | = concentration of USP Parthenolide RS in the Standard solution (mg/mL) |
| V | = | = final volume of the Sample stock solution (mL) |
| W | = | = weight of Powdered Feverfew used to prepare the Sample stock solution (mg) |
| D | = | = dilution factor to prepare the Sample solution from the Sample stock solution |
Acceptance criteria:
NLT 0.2% on the dried basis
CONTAMINANTS
• Heavy Metals 
231
:
NMT 20 ppm
231:
NMT 20 ppm
• Articles of Botanical Origin, Pesticide Residues 561:
Meets the requirements
561:
Meets the requirements
• Microbial Enumeration Tests 2021:
The total aerobic bacterial count does not exceed 104 cfu/g, and the total combined molds and yeasts count does not exceed 102 cfu/g.
2021:
The total aerobic bacterial count does not exceed 104 cfu/g, and the total combined molds and yeasts count does not exceed 102 cfu/g.
• Microbiological Procedures for Absence of Specified Microorganisms 2022:
It meets the requirements of the tests for the absence of Salmonella species, Escherichia coli, and Staphylococcus aureus.
2022:
It meets the requirements of the tests for the absence of Salmonella species, Escherichia coli, and Staphylococcus aureus.
SPECIFIC TESTS
• Loss on Drying 731:
Dry 1.0 g of Powdered Feverfew at 105 for 1 h: it loses NMT 10.0% of its weight.
731:
Dry 1.0 g of Powdered Feverfew at 105 for 1 h: it loses NMT 10.0% of its weight.
• Articles of Botanical Origin, Total Ash 561:
NMT 12.0%
561:
NMT 12.0%
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers, protected from light and moisture.
• Labeling:
The label states the Latin binomial and, following the official name, the part of the plant source from which the article was derived.
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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 1290