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.
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.
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 
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)
Calculate the percentage of the labeled amount of Guggul Extract taken:
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.
•  Weight Variation 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.
•  Absence of Specified Microorganisms 2022: It meets the requirements of the tests for absence of Salmonella species and Escherichia coli.
•  Residual Solvents 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.
•  USP Reference Standards 11
USP Guggulsterone Z RS
USP Purified Guggul Extract RS
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Topic/Question Contact Expert Committee
Monograph Maged H. Sharaf, Ph.D.
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2021 Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison
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2022 Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison
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