猪胆粉

English text reference: Chinese Pharmacopoeia (2020 Edition)

Overview

Pig Bile Powder is the dried bile of Sus scrofa domestica Brisson (Fam. Suidae).

Processing

The bile is collected from pigs, filtered, dried, and powdered.

Description

Pig Bile Powder is yellow or grayish-yellow powder. It has a slight fishy odor, a bitter taste, and is hygroscopic.

Identification

Take 0.1g of the fine powder, add 5ml of 10% sodium hydroxide solution, heat at 120°C for 4 hours, cool, adjust the pH value to 2-3 by adding hydrochloric acid, shake well. Extract with four 10ml portions of ethyl acetate, combine the extracts, evaporate to dryness. Dissolve the residue in 10ml of ethanol as the test solution. Take an appropriate amount of deoxycholic acid CRS, dissolve in ethanol to produce a solution containing 1mg per ml as the Reference solution. Carry out the method for thin layer chromatography<0502>, using the upper layer solution of a newly prepared mixture of isooctane, ether, glacial acetic acid, n-butanol, and water (10:5:5:3:1) as the coating substance and a mixture of petroleum ether(60-90°C)and ether(4:5)as the mobile phase. Apply separately to the plate 2μl of each of the above two solutions. After developing and removal of the plate,dry in air. Spray with a 10% solution of sulfuric acid in ethanol, heat at 105°C to the spots clear. Examine under daylight and ultraviolet light at 365nm. The spots or fluorescent spots in the chromatogram obtained with the test solution correspond in position and colour to the spots in the chromatogram obtained with the Reference solution.

Examination

Ox Bile, Sheep Bile

Take 0.1g each of Ox Bile and Sheep Bile, prepare the test solutions according to the method described under "Identification" from the step of "add 5ml of 10% sodium hydroxide solution", and prepare the reference solutions of the corresponding medicinal materials in the same way. Carry out the method for thin layer chromatography<0502>, using the same procedure as described under "Identification". The spots in the chromatogram obtained with the test solution should not correspond in position and colour to the spots in the chromatogram obtained with the reference solutions of Ox Bile and Sheep Bile.

Reducing sugars

Take 10mg of the powder, dissolve in 2ml of water, add a few drops of α-naphthol ethanol solution (1→50), shake well, add about 0.5ml of sulfuric acid slowly along the tube wall, the interface of the two liquids should not show a purple-red ring.

Foreign organic matter

Take 10mg of the powder, dissolve in 2ml of water, centrifuge or filter, take the insoluble matter, observe under a microscope, there should be no plant tissue, animal tissue, or starch.

Water

Take about 0.3g of the powder, accurately weigh, carry out the determination of water content according to the method for water determination<0832, method 3>, the water content should not be more than 10.0%.

Assay

Carry out the determination by high performance liquid chromatography<0512>.

Chromatographic conditions and system suitability test

Use octadecylsilane bonded silica gel as the filler (column length 250mm; inner diameter 4.6mm); use a mixture of methanol and 0.03mol/L sodium dihydrogen phosphate solution (70:30) as the mobile phase (adjust the pH value to 4.4 with phosphoric acid); detect at a wavelength of 200nm. The theoretical plate number calculated from the peak of tauroursodeoxycholic acid should not be less than 3000.

Preparation of reference solution

Take an appropriate amount of tauroursodeoxycholic acid CRS, accurately weigh, dissolve in methanol to produce a solution containing 0.5mg per ml, and set aside.

Preparation of test solution

Take about 0.5g of the powder, accurately weigh, place it in a 50ml volumetric flask, add 20ml of methanol, ultrasonicate (power 500W, frequency 40kHz) for 20 minutes, cool, add methanol to the mark, shake well, filter, and take the filtrate.

Assay method

Accurately aspirate 20μl each of the reference solution and the test solution, inject into the liquid chromatograph, and determine the content.

Calculate the content of tauroursodeoxycholic acid (C26H45O6NS) in the dried powder, which should not be less than 2.0%.

Property

Cold.

Flavor

Bitter.

Meridian tropism

Liver, gallbladder, lung, and large intestine meridians.

Actions

It clears heat and moistens dryness, stops coughing and relieves asthma, and detoxifies.

Indications

It is used for cough, asthma, fever with thirst, red eyes, sore throat, jaundice, diarrhea, dysentery, constipation, and boils and swelling.

Dosage

0.3-0.6g. For external use, use an appropriate amount.

Administration

Taken orally or made into pills or powder. Grind into powder or mix with water and apply to the affected area.

Storage

Store in a sealed container, protected from light, in a cool and dry place.

猪胆粉

Text reference: Chinese Pharmacopoeia (2015 Edition)

Overview

Pig Gall Powder is the dried bile of Sus scrofa domestica Brisson (Fam. Suidae).

Processing

Take pig bile, filter, dry and pulverize.

Description

Yellow, greyish-yellow powder. Odour, slightly stinking. Taste, bitter, easily moistened.

Identification

To 0.1 g of the fine powder, add 5 ml of 10% sodium hydroxide solution, heat at 120℃ for 4 hours, and cool. Adjust to pH 2-3 with hydrochloride acid, mix well. Extract by shaking with four 10-ml quantities of ethyl acetate, evaporate the combined extracts to dryness. Dissolve the residue in 10-ml of ethanol as the test solution. Dissolve a quantity of hyodeoxycholic acid CRS in ethanol 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 the upper layer of a freshly prepared mixture of isooctane, ether, glacial acetic acid, n-butanol and water (10 : 5 : 5 : 3 : 1) as the mobile phase. Apply separately 2 μl of each of the test solution and the reference solution to the plate. After developing and removal of the plate, dry in air, spray with a 10% solution of sulfuric acid in ethanol, heat at 105℃ to visualize clearly. Examine in daylight and under ultraviolet light at 365 nm. The spots in the chromatogram obtained with the test solution correspond in position and colour to the spots in the chromatogram obtained with the reference solution.

Examination

Fellis Bovis, Fellis Caprae seu Ovis

Take 0.1 g each of Fellis Bovis reference drug and Fellis Caprae seu Ovis reference drug, produce two reference drug solutions in the same manner as preparation of the test solution under Identification, beginning at the words "add 5 ml of 10% sodium hydroxide...". Carry out the method for thin layer chromatography <0502>, using silica gel G as the coating substance. apply separately to the plate 2 μl each of the test solution obtained under Identification and the above two reference drug solutions. Developing and visualizing in the same manner as described under the test of Identification. The spots in the chromatogram obtained with the test solution should not be corresponding in position and colour to the spots in the chromatogram obtained with the reference drug solutions.

Reducing sugars

Dissolve 10 mg of the powder in 2 ml of water, add several drops of α-naphthol in ethanol (1→50), mix well, add dropwise 0.5 mil of sulfuric acid along the tube wall, a purplish-red ring is not visible at the junction of the two layers.

Foreign organic matter

Dissolve 10 mg of the powder in 2 ml of water, centrifuge or filter. Examine the residue under the microscope. No plant. animal tissues or starch is visible.

Water

Weigh accurately 0.3 g of the powder, carry out the method for determination of water <0832, method 3>, not more than 10.0 per cent.

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 (250 mm × 4.6 mm and a mixture of methanol and 0.03 mol/L sodium dihydrogenphosphate adjust to pH 4.4 with phosphoric acid) (70 : 30) as the mobile phase. As detector a spectrophotometer set at 200 nm. The number of theoretical plates of the column is not less than 3000, calculated with reference to the peak of taurohyodeoxycholic acid.

Reference solution

Dissolve a quantity of taurohy-odeoxycholic acid CRS, accurately weighed, in methanol to prepare a solution containing 0.5 mg per ml.

Test solution

Weigh accurately 0.5 g of the powder to a 50 ml volumetric flask, add 20 ml of methanol. Ultrasonicate (power 500 W, frequency 40 kHz) for 20 minutes, cool and dilute with methanol to volume, mix well and filter, 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, determine and calculate the content.

It contains not less than 2.0 per cent of taurohyodeoxycholic acid (C26H45O6NS), calculated with reference to the dried drug.

Property and Flavor

Cold; bitter. Liver, gallbladder, lung, large intestine meridians.

Actions

To clear heat, moisten dryness, suppress cough, relieve panting, and remove toxin. Used for whooping cough, asthma, febrile disease with dryness thirst, red eyes, throat bi disorder, jaundice, diarrhea, dysentery, constipation, abscess, sore, swelling skin infections.

Administration and dosage

0.3-0.6 g, taken with water or used in pills and powder; Appropriate amount for topical application, ground into powder, or mixed with water for applying to the affected area.

Storage

Preserve in tightly closed container, and protect from light and stored in a cool and dry place.