Powdered Aloe-Aloe Pulverata (barbaloin)

Powdered Aloe

Aloe Pulverata

Powdered Aloe is the powder of Aloe.
It contains not less than 4.0z of barbaloin, calculated on the basis of dried material.

Description:

Powdered Aloe occurs as a dark brown to yellowish dark brown powder. It has a characteristic odor and an extremely bitter taste.
Under a microscope, Powdered Aloe, immersed in olive oil or liquid paraffin, reveals greenish yellow to reddish brown, angular or rather irregular fragments.

Identification:

(1) Dissolve 0.5 g of Powdered Aloe in 50 mL of water by warming. After cooling, add 0.5 g of siliceous earth, and filter. Perform the following tests with the filtrate as the sample solution.
(i) Dissolve 0.2 g of sodium tetraborate decahydrate in 5 mL of the sample solution by warming in a water bath. Add a few drops of this solution into 30 mL of water, and shake: a green fluorescence is produced.
(ii) Shake 2 mL of the sample solution with 2 mL of nitric acid: a yellow-brown color which changes gradually to green is produced. Then warm this colored solution in a water bath: the color of the solution changes to red-brown.
(2) To 0.2 g of Powdered Aloe add 10 mL of methanol, shake for 5 minutes, filter, and use the filtrate as the sample solution. Separately, dissolve 1 mg of barbaloin for thin layer chromatography in 1 mL of methanol, and use this solution as the standard solution. Perform the test with these solutions as directed under Thin-layer Chromatography. Spot 10 mL each of the sample solution and standard solution on a plate of silica gel for thin-layer chromatography. Develop the plate with a mixture of ethyl acetate, acetone, water and acetic acid (100) (20:5:2:2) to a distance of about 10 cm, and air-dry the plate. Examine under ultraviolet light (main wavelength: 365 nm): one spot among several spots from the sample solution has the same color tone and the same Rf value with the red fluorescent spot from the standard solution.

Purity:

(1) Resin.Warm 0.5 of Powdered Aloe with 10 mL of diethyl ether on a water bath, and filter. Wash the residue and the filter paper with 3 mL of diethyl ether. Combine the filtrate and the washing, and evaporate the diethyl ether: the mass of the residue does not exceed 5.0 mg.
(2) Ethanol-insoluble substances.Boil 1.0 g of Powdered Aloe with 50 mL of ethanol (95) on a water bath for 30 minutes under a reflux condenser. Filter the warm mixture through a tared glass filter (G4), and wash the residue on the filter with ethanol (95) until the last washing becomes colorless. Dry the residue at 105oC for 5 hours, and weigh: the mass of the residue is not more than 0.10 g.

Loss on drying:

Not more than 12.0z.

Total ash:

Not more than 2.0z.

Extract content:

Water-soluble extract: not less than 40.0z.

Assay:

Weigh accurately about 0.1 g of Powdered Aloe, add 40 mL of methanol, and heat under a reflex condenser on a water bath for 30 minutes. After cooling, filter, and add methanol to the filtrate to make exactly 50 mL. Pipet 5 mL of the solution, add methanol to make exactly 10 mL, and use this solution as the sample solution. Separately, weigh accurately about 10 mg of barbaloin for assay, previously dried in a desiccator (in vacuum, phosphorus (V) oxide) for 24 hours, add 40 mg of oxalic acid dihydrate, and dissolve in methanol to make exactly 100 mL. Pipet 5 mL of the solution, add methanol to make exactly 10 mL, and use this solution as the standard solution. Perform the test with exactly 5 mL each of the sample solution and standard solution as directed under Liquid Chromatography <2.01> according to the following conditions, and determine the peak areas of barbaloin, AT and AS, of both solutions.
Amount (mg) of barbaloin MS × AT/AS × 1/2
MS: Amount (mg) of barbaloin for assay
Operating conditions.
Detector: An ultraviolet absorption photometer (wave length: 360 nm).
Column: A stainless steel column about 6 mm in inside diameter and about 15 cm in length, packed with octadecyl silanized silica gel for liquid chromatography (5 mm in particle diameter).
Column temperature: A constant temperature of about 30oC.
Mobile phase: A mixture of water, acetonitrile and acetic acid (100) (74:26:1).
Flow rate: Adjust the flow rate so that the retention time of barbaloin is about 12 minutes.
System suitability.
System performance: To about 10 mg of barbaloin for assay add 40 mg of oxalic acid dihydrate, and dissolve in methanol to make 100 mL. To 5 mL of the solution add 1 mL of a solution of ethenzamide in methanol (1 in 2000) and methanol to make 10 mL. When the procedure is run with 5 mL of this solution under the above operating conditions except the wavelength of 300 nm, barbaloin and ethenzamide are eluted in this order with the resolution between these peaks being not less than 2.0.
System repeatability: When the test is repeated 6 times with 5 mL of the standard solution under the above operating conditions, the relative standard deviation of the peak area of barbaloin is not more than 1.5z.

Containers and storage:

Containers.Tight containers.

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