Cascara Sagrada
(kas kar' a sa gra' da).
DEFINITION
Cascara Sagrada is the dried bark of Frangula purshiana (DC.) J. G. Cooper (syn. Rhamnus purshiana DC) (Fam. Rhamnaceae). It yields NLT 7.0% of total hydroxyanthracene derivatives, calculated as cascaroside A, and calculated on the dried basis. NLT 60% of the total hydroxyanthracene derivatives consists of cascarosides, calculated as cascaroside A.
[Note—Collect Cascara Sagrada not less than one year before use. ]
IDENTIFICATION
• A.
Sample:
100 mg of powdered Cascara Sagrada
Analysis:
Add the Sample to 10 mL of hot water, shake the mixture occasionally until it is cold, filter, dilute the filtrate with water to 10 mL, and add 10 mL of 6 N ammonium hydroxide.
Acceptance criteria:
An orange color is produced.
• B.
Sample:
A portion of Cascara Sagrada
Analysis:
Treat the Sample with 6 N ammonium hydroxide.
Acceptance criteria:
It becomes red to reddish brown in color.
• C.
Sample:
100 mg of powdered Cascara Sagrada
Analysis:
Macerate the Sample with 1 mL of alcohol, add 10 mL of water, boil the mixture, then cool, filter, and shake the filtrate with 10 mL of ether: a greenish-yellow ether layer separates. Shake 3 mL of the ether layer with 3 mL of 6 N ammonium hydroxide, and dilute the separated ammonia solution with 20 mL of water.
Acceptance criteria:
A distinct orange-pink color remains.
COMPOSITION
• Content of Total Hydroxyanthracene Derivatives
Perform all extractions by shaking vigorously, and allow all phases to separate completely before transferring. Entrainment of aglycones into the aqueous phase, as indicated by a value of less than 2.6 for the ratio of the absorbance of the final solution at 515 nm to that at 440 nm, may lead to false results.
Throughout this procedure, use 1 N sodium hydroxide that is prepared without added barium ions as directed in Reagents, Indicators, and Solutions—Volumetric Solutions.
Ferric chloride solution:
1 g/mL of ferric chloride in water
Sample stock solution:
Add 1 g of Cascara Sagrada to 70 mL of boiling water, boil for several min, with stirring. Allow to cool, and transfer with the aid of water to a 100-mL volumetric flask. Dilute with water to volume, mix, and filter through suitable filter paper.
Sample solution:
Pipet 10 mL of Sample stock solution into a separatory funnel containing 5 mL of water and 2 drops of 1 N hydrochloric acid. Extract with 40 mL of methylene chloride, and transfer the lower layer to a second separatory funnel. Add 10 mL of water to the second separatory funnel, and shake. Allow to separate, discard the lower layer, and transfer the water layer to the first separatory funnel. Extract the combined water layers with 40 mL of methylene chloride, and transfer the lower layer to the second separatory funnel. Add 10 mL of water to the second separatory funnel, and shake. Allow to separate, and discard the lower layer. Transfer the combined water layers, with the aid of water, to a 50-mL volumetric flask, dilute with water to volume, and mix.
Instrumental conditions
Mode:
Visible
Analytical wavelength:
515 nm
Cell:
1 cm
Blank:
Methanol
Analysis
Sample:
Sample solution
Pipet 15 mL of Sample solution into a flask containing 2 mL of Ferric chloride solution and 12 mL of hydrochloric acid. Attach a condenser arranged for refluxing, and heat for 3 h by keeping the flask immersed in boiling water or continuously exposed to steam heat. Cool, wash down the condenser, and transfer to a separatory funnel with the aid of 4 mL of 1 N sodium hydroxide and five 6-mL portions of water. Extract with 20 mL of methylene chloride, and transfer the lower layer to another separatory funnel. Repeat the extraction with three additional 20-mL portions of methylene chloride, wash the combined methylene chloride extracts with two 10-mL portions of water, shaking each time for 2 min, and discard the water washings. Transfer the washed methylene chloride extract to a 100-mL volumetric flask, dilute with methylene chloride to volume, and mix. Evaporate a 15.0-mL portion carefully on a water bath to dryness, and dissolve the residue in 10.0 mL of a 5-mg/mL solution of magnesium acetate in methanol.
Calculate the quantity, in mg, of total hydroxyanthracene derivatives (THD) in the portion of Cascara Sagrada taken:
THD = AU × F
| AU | = | = absorbance of the Sample solution |
| F | = | = conversion factor, 138. [Note—This conversion factor considers an absorptivity of 16.1 for cascaroside A and the dilutions to prepare the solution for analysis. ] |
Calculate the percentage of of total hydroxyanthracene derivatives, calculated as cascaroside A:
Result = (THD/W) × 100
| W | = | = weight of Cascara Sagrada taken to prepare the Sample stock solution (mg) |
Acceptance criteria:
NLT 7.0%, calculated on the dried basis
• Content of Cascarosides
Perform all extractions by shaking vigorously, and allow all phases to separate completely before transferring. Entrainment of aglycones into the aqueous phase, as indicated by a value of less than 2.7 for the ratio of the absorbance of the final solution at 515 nm to that at 440 nm, may lead to false results.
Throughout this procedure, use 1 N sodium hydroxide that is prepared without added barium ions as directed in Reagents, Indicators, and Solutions—Volumetric Solutions.
Ferric chloride solution and Sample stock solution:
Prepare as directed in the Assay for Content of Total Hydroxyanthracene Derivatives.
Sample solution:
Pipet 10 mL of Sample stock solution into a separatory funnel containing 5 mL of water and 2 drops of 1 N hydrochloric acid. Extract with 40 mL of methylene chloride, and transfer the lower layer to a second separatory funnel. Add 10 mL of water to the second separatory funnel, and shake. Allow to separate, discard the lower layer, and transfer the water layer to the first separatory funnel. Extract the combined water layers with 40 mL of methylene chloride, and transfer the lower layer to the second separatory funnel. Add 10 mL of water to the second separatory funnel, and shake. Allow to separate, discard the lower layer, and transfer the water layer to the first separatory funnel. Extract the combined aqueous phase with 30 mL of clear, freshly prepared, water-saturated ethyl acetate, and transfer the water layer to another separatory funnel. Repeat the extraction with two additional 30-mL portions of the freshly prepared, water-saturated ethyl acetate. Add 5 mL of water to the combined ethyl acetate extracts, shake, allow the phases to separate, discard the ethyl acetate extracts, and add 30 mL of the freshly prepared, water-saturated ethyl acetate to the water wash. Shake, allow the phases to separate, and discard the ethyl acetate phase. Transfer the combined aqueous phases, with the aid of water, to a 50-mL volumetric flask. Dilute with water to volume.
Instrumental conditions
Mode:
Visible
Analytical wavelength:
515 nm
Cell:
1 cm
Blank:
Methanol
Analysis
Proceed as directed for Analysis in Content of Total Hydroxyanthracene Derivatives, except to evaporate a 20.0-mL portion of the methylene chloride solution instead of 15.0 mL.
Sample:
Sample solution
Determine the absorbance and calculate the percentage of cascarosides with respect to the content of total hydroxyanthracene derivatives in the portion of Cascara Sagrada taken:
Result = (AU/THD) × F × 100
| AU | = | = absorbance of the Sample solution |
| THD | = | = weight of total hydroxyanthracene derivatives (mg) |
| F | = | = conversion factor, 103.5. [Note—This conversion factor considers an absorptivity of 16.1 for cascaroside A and the dilutions to prepare the solution for analysis. ] |
Acceptance criteria:
NLT 60% of the total hydroxyanthracene derivatives consists of cascarosides, calculated as cascaroside A on the dried basis
SPECIFIC TESTS
• Botanic Characteristics
Macroscopic
Cascara Sagrada:
The bark is usually in the form of flattened or transversely curved pieces, occasionally in quills of variable length and from 1 to 5 mm in thickness. The outer surface is brown, purplish brown, or brownish red, longitudinally ridged, with or without grayish or whitish lichen patches, sometimes with numerous lenticels and occasionally with moss attached. The inner surface is longitudinally striate, light yellow, weak reddish brown, or moderate yellowish brown. The fracture is short with projections of phloem fiber bundles in the inner bark.
Powdered Cascara Sagrada:
The powder is moderate yellowish brown to dusky yellowish orange.
Microscopic
Cascara Sagrada:
The transverse section of the bark shows a yellowish-brown, purple, or reddish-brown cork of up to 10 or more rows of small cells; stone cells in yellowish, tangentially elongated groups of 20–50 cells in the cortex, pericycle, and outer phloem regions; phloem rays 1–4 cells wide, 15–25 cells deep, frequently diagonal or curved, forming converging groups; phloem fibers in small bundles, more or less surrounded by crystal fibers and located between the phloem rays; parenchyma with brown walls and containing starch grains and calcium oxalate crystals.
Powdered Cascara Sagrada:
It shows numerous broken phloem fiber bundles with accompanying crystal fibers containing monoclinic prisms of calcium oxalate; stone cells more or less adherent, in small groups with thick, finely lamellated and porous walls; fragments of reddish-brown to yellow cork; masses of parenchyma and phloem ray cells colored reddish brown to orange upon the addition of a solution of an alkali; starch grains spheroidal, up to 8 µm in diameter; calcium oxalate in monoclinic prisms or rosette aggregates from 6 to 20 µm in diameter, occasionally up to 45 µm in diameter.
• Water Determination, Method III, Procedure for Articles of Botanical Origin 
921
:
Dry a sample at 105
for 5 h: it loses NMT 12.0% of its weight.
921:
Dry a sample at 105 for 5 h: it loses NMT 12.0% of its weight.
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 |
USP35–NF30 Page 2518