熟地黄

English text reference: Chinese Pharmacopoeia (2020 Edition)

Overview

Prepared Rehmannia Root is the processed product of Rehmannia glutinosa Libosch. (Fam. Scrophulariaceae).

Processing

(1) Take raw dihuang, according to the wine stewing method (general rule 0213) stewed until the wine sucked out, take out, drying until the mucus of the outer skin is slightly dry, cut thick slices or blocks, drying, that is, obtained. For every 100 kg of raw dihuang, use 30-50 kg of yellow wine.

(2) Take raw dihuang, according to the method of steaming (Tongzhi 0213) steamed to black moist, take out, sunshine to about eighty percent dry, cut thick slices or blocks, dry, that is, get.

Description

Pieces or fragments of irregular shape, of variable size and thickness. Surface black and glossy, with a large amount of sticky substance. Texture soft and slightly tough, not easily broken; fracture black and glossy. Odour, slight; taste, sweet.

Identification

To 1 g of the powder add 50 ml of 80% methanol, treat with ultrasound for 30 minutes, filter, evaporate the filtrate to dryness, dissolve the residue in 5 ml of water. Extract with four 10 ml portions of water-saturated n-butanol, combine the n-butanol extracts, evaporate to dryness. Dissolve the residue in 2 ml of methanol as the test solution. Dissolve catalpol CRS in methanol to produce a solution containing 1 mg per ml as the Reference solution. Carry out the method for thin layer chromatography<0502>, using silica gel G as the coating substance and a mixture of ethyl acetate-methanol-formic acid(16:0.5:2)as the mobile phase. Apply separately to the plate 5 μl of the test solution and 2 μl of the Reference solution. After developing and removal of the plate, dry in air. Spray with a 0.1% solution of 2,2-diphenyl-1-picrylhydrazyl in anhydrous ethanol. Dry. The spot in the chromatogram obtained with the test solution corresponds in position and colour to the spot in the chromatogram obtained with the Reference solution.

Examination

Same as Rehmannia.

Extractives

Same as Rehmannia.

Assay

Determine by high-performance liquid chromatography <0512>.

Chromatographic conditions and system suitability test

Use octadecylsilane-bonded silica gel as the filler; use methanol-0.1% phosphoric acid solution (5:95) as the mobile phase, and detect at a wavelength of 203 nm. The theoretical plate number calculated based on the peak of Rehmannioside D should not be less than 5000.

Preparation of reference solution

Take an appropriate amount of Rehmannioside D reference substance, accurately weigh it, add 25% methanol to make a solution containing 70 μg per 1 ml.

Preparation of test solution

Take this product and cut it into small pieces of about 5 mm. After drying under reduced pressure at 80°C for 24 hours, grind it into coarse powder. Take about 1 g, accurately weigh it, place it in a stoppered conical flask, accurately add 25% methanol 25 ml, weigh it, perform ultrasonic treatment (power 400 W, frequency 50 kHz) for 1 hour, let it cool, weigh it again, make up for the weight loss with 25% methanol, shake well, centrifuge at high speed for 10 minutes, take the supernatant and filter it, and take the filtrate.

Assay method

Accurately take 10 μl of the reference solution and the test solution, inject them into the liquid chromatograph, and determine the content.

The content of Rehmannioside D (C27H42O20) in this product should not be less than 0.050%.

Property

Slightly warm.

Toxicity

None.

Flavor

Sweet.

Meridian tropism

Liver and kidney meridians.

Actions

Nourish blood and nourish yin, tonify essence and fill the marrow.

Indications

Used for blood deficiency and withered yellow, palpitations and flustered, irregular menstruation, excessive menstrual flow, liver and kidney yin deficiency, soreness and weakness of the waist and knees, steaming bone and tidal heat, night sweats and spermatorrhea, internal heat and thirst, dizziness, tinnitus, premature graying of hair.

Dosage

9-15 g.

Administration

None.

Storage

Store in a well-ventilated and dry place.

熟地黄

Text reference: Chinese Pharmacopoeia (2015 Edition)

Overview

The drug is the processed Rehmanniae Radix.

Procedure

To stew the Rehmanniae Radix as described under the method for stewing with wine <0213>, until the wine is absorbed entirely, take out, dry in the sun until the mucilage in bark is slightly dried, cut into thick slices or pieces, and dry thoroughly.

To each 100 kg of Rehmanniae Radix add 30-50 kg of yellow rice wine.

To steam the Rehmannise Radix as described under the method for steaming <0213> until it becomes blackish and shiny, take out, dry in the sun to be eighty percent dried, cut into thick slices or pieces, and dry thoroughly.

Description

Occurring in irregular slices and pieces, broken lumps, varying in size and thickness. Externally black, lustrous, more sticky. Texture soft and flexible, not easy to break, fracture black, lustrous. Odour, slight; taste, sweet.

Identification

To 1 g of the powder add 50 ml of 80% methanol, ultrasonicate for 30 minutes, filter. Evaporate the filtrate to dryness, dissolve the residue in 5 ml of water. Extract with four 10-ml quantities of n-butanol saturated with water by shaking, combine the n-butanal solutions, evaporate to dryness. Dissolve the residue in 2 ml of methanol as the test solution. Dissolve a quantity of verbascoside CRS in methanol to produce a solution containing 1 mg per ml as the reference solution. Carry out the method for thin layer chromatography <0502>, using silica gel G as the coating substance and a mixture of ethyl acetate, methanol and formic acid (16 : 0.5 : 2) as the mobile phase. Apply separately 5 μl of the test solution and 2 μl of the reference solution to the plate. After developing and removal of the plate. dry in air. Soak the plate briefly in a 0.1% solution of 2, 2-diphenyl-1-picrylhydrazyl in dehydrated ethanol, take out and dry in air. The spot in the chromatogram obtained with the test solution corresponds in position and colour to the spot in the chromatogram obtained with the reference solution.

Examination

Water

As required for Rehmanniae Radix.

Total ash

As required for Rehmanniae Radix.

Acid-insoluble ash

As required for Rehmanniae Radix.

Extractives

As required for Rehmanniae Radix.

Assay

Carry out the method for high performance liquid chromatography <0512>.

Chromatographic system and system suitability

Use octadecylsilane bonded silica gel as the stationary phase and a mixture of acetonitrile and 0.1% solution of acetic acid (16 : 84) as the mobile phase. As detector spectrophotometer set at 334 nm. The number of theoretical plates of the column is not less than 5000, calculated with reference to the peak of verbascoside.

Reference solution

Dissolve a quantity of verbascoside CRS, accurately weighed, in mobile phase to prepare a solution containing 10 μg per ml as the reference solution.

Test solution

Weigh accurately 2 g of the very coarse powder to a round-bottomed flask, add accurately 100 ml of methanol and weigh. Heat under reflux for 30 minutes, cool and weigh again, replenish the loss of solvent with methanol, mix well and filter. Measure accurately 50 ml of the successive filtrate and recover the solvent in vacuum to nearly dryness. Dissolve the residue with the mobile phase and transfer to a 10 ml volumetric flask and dilute with the mobile phase to the volume, mix well, filter and use the successive filtrate as the test solution.

Procedure

Inject accurately 20 μl of each of the reference solution and the test solution, respectively, into the column, and calculate the content.

It contains not less than 0.020 per cent of verbascoside (C29H36O15), calculated with reference to the dried drug.

Property and Flavor

Mild warm; sweet. Liver and kidney meridians.

Actions

To nourish blood, replenish yin, replenish the essence and the marrow. Blood deficiency, sallow complexion, palpitations, fearful throbbing, menstrual irregularities, flooding and spotting, liver-kidney yin deficiency, soreness and weakness in the lower back and knees, bone-steaming and tidal fever, night sweating seminal emission, interior heat, wasting-thirst, dizziness. tinnitus, and premature greying.

Administration and dosage

9-15 g.

Storage

Preserve in a ventilated and dry place.