Guggul Tablets
DEFINITION
Guggul Tablets are prepared from Native Guggul Extract or Purified Guggul Extract. Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of Extract, calculated as the sum of guggulsterones E and Z.
IDENTIFICATION
• A. Thin-Layer Chromatographic Identification Test
Standard solution:
10 mg/mL of USP Purified Guggul Extract RS, with heating, in acetonitrile
Sample solution:
Powder and transfer a portion of the Tablets equivalent to 100 mg of Extract to a conical flask. Extract three times, each with 25 mL of acetonitrile, in a 55
water bath for 15 min, stirring with a magnetic stirrer, and filter. Evaporate the combined extracts to dryness in a vacuum between 45 and 50, dissolve the residue in 10 mL of acetonitrile, centrifuge, and use the clear supernatant.
water bath for 15 min, stirring with a magnetic stirrer, and filter. Evaporate the combined extracts to dryness in a vacuum between 45 and 50, dissolve the residue in 10 mL of acetonitrile, centrifuge, and use the clear supernatant.
Chromatographic system
Developing solvent system:
A mixture of hexane and ethyl acetate (6:4)
Adsorbent:
0.25-mm layer of chromatographic silica gel mixture, typically 20 cm in length
Application volume:
10 µL
Analysis
Samples:
Standard solution and Sample solution
Apply the Samples as bands to a suitable plate. Use a saturated chamber. Develop until the solvent front has moved about about three-fourths the length of the plate, dry the plate, and examine under UV light at 254 nm.
Acceptance criteria:
The chromatogram of the Sample solution exhibits bands at RF values of about 0.38 and 0.47, due to guggulsterone E and Z, respectively. Both bands correspond in RF to bands in the chromatogram from the Standard solution.
• B. HPLC Identification Test
Analysis:
Proceed as directed in the test for Content of Guggulsterones E and Z.
Acceptance criteria:
The chromatogram of the Sample solution exhibits peaks for guggulsterones E and Z at retention times that correspond to those of Standard solution A.
STRENGTH
• Content of Guggulsterones E and Z
Mobile phase:
A mixture of acetonitrile and water (45:55)
Standard solution A:
10 mg/mL of USP Purified Guggul Extract RS, with heating, in acetonitrile. Pass the solution through a filter of 0.45-µm pore size before injection.
Standard solution B:
0.1 mg/mL of USP Guggulsterone Z RS in acetonitrile. Pass the solution through a filter of 0.45-µm pore size before injection.
Sample solution:
Weigh and finely powder NLT 20 Tablets. Transfer a weighed amount of the powder, equivalent to about 10 mg of guggulsterones E and Z, to a conical flask, and extract five times, each with a 20-mL portion of acetonitrile, shake for 1 min, and reflux in a water bath for 30 min, stirring with a magnetic stirrer. Evaporate the combined extracts to dryness in a vacuum at 45–50. Dissolve the residue in 50.0 mL of acetonitrile, and pass through a filter of 0.45-µm pore size before injection.
–50. Dissolve the residue in 50.0 mL of acetonitrile, and pass through a filter of 0.45-µm pore size before injection.
Chromatographic system
Mode:
LC
Detector:
UV 242 nm
Column:
4.6-mm × 25-cm; 5-µm packing L1
Flow rate:
2.0 mL/min
Injection size:
20 µL
Column temperature:
27 ± 1
System suitability
Samples:
Standard solution A and Standard solution B [Note—The relative retention times for guggulsterones E and Z are about 0.69 and 1.0, respectively. ]
Suitability requirements
Chromatogram similarity:
The chromatogram from Standard solution A is similar to the reference chromatogram provided with the lot of USP Purified Guggul Extract RS being used.
Resolution:
NLT 2.0 between the guggulsterone Z peak and the peak before, Standard solution A
Tailing factor:
NMT 1.5 for the guggulsterone Z peak, Standard solution B
Relative standard deviation:
NMT 2.0% for the guggulsterone Z peak (replicate injections), Standard solution B
Analysis
Calculate the percentage of the labeled amount of Guggul Extract taken:
Samples:
Standard solution A, Standard solution B, and Sample solution
Allow Standard solution A to elute for NLT two times the retention time of guggulsterone Z, as determined in Standard solution B. Using the chromatogram of Standard solution A and the reference chromatogram provided with the lot of USP Purified Guggul Extract RS being used, identify the retention times of the peaks corresponding to guggulsterone E and guggulsterone Z.
Calculate the content of guggulsterones E and Z as guggulsterone Z in the portion of Tablets taken:
CI = (rU/rS) × CS × V
| rU | = | = sum of the peak responses of guggulsterones E and Z from the Sample solution |
| rS | = | = peak response of guggulsterone Z from Standard solution B |
| CS | = | = concentration of USP Guggulsterone Z RS in Standard solution B (mg/mL) |
| V | = | = final volume of the Sample solution (mL) |
Result = CI × (AWT/W) × (100/LE) × (100/L)
| CI | = | = content of guggulsterones E and Z in the portion of Tablets taken (mg) |
| AWT | = | = average weight of Tablets (mg) |
| W | = | = weight of the powdered Tablets taken (mg) |
| LE | = | = labeled percentage of the sum of guggulsterones E and Z in the Extract used to prepare the Tablets |
| L | = | = label claim of Extract (mg/Tablet) |
Acceptance criteria:
90.0%–110.0% of the labeled amount of Extract, calculated as the sum of guggulsterones E and Z
PERFORMANCE TESTS
• Disintegration and Dissolution 
2040
:
It meets the requirement for Disintegration only; 30 min, the use of the disk being omitted.
2040:
It meets the requirement for Disintegration only; 30 min, the use of the disk being omitted.
• Weight Variation 2091:
Meet the requirements
2091:
Meet the requirements
CONTAMINANTS
• Microbial Enumeration Tests 2021:
The total aerobic microbial count does not exceed 104 cfu/g, and the total combined yeasts and molds count does not exceed 103 cfu/g.
2021:
The total aerobic microbial count does not exceed 104 cfu/g, and the total combined yeasts and molds count 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.
• Residual Solvents 467:
Meets the requirements
467:
Meets the requirements
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers, protected from light and moisture, and store at room temperature.
• Labeling:
The label states the Latin binominal and, following the official name, the article from which the Tablets were prepared. The label also indicates the amount of Extract, in mg/Tablet, and the content, in mg, of guggulsterones E and Z per 100 mg of Extract.
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 1353
Pharmacopeial Forum: Volume No. 34(4) Page 1004