雄黄

English text reference: Chinese Pharmacopoeia (2020 Edition)

Overview

Realgar is a mineral of the sulfide class, belonging to the realgar group. It mainly contains arsenic disulfide (As2S2). After mining, impurities are removed.

Description

Realgar is a block or granular aggregate, irregular in shape. It is deep red or orange-red in color, with pale orange-red streaks and diamond-like luster on the crystal surface. It is brittle and easily broken, with a resin-like luster on the fracture surface. It has a slight peculiar odor and a mild taste. The powdered ore is powdery or powdery aggregate, loose and brittle, easily crushed into powder by hand, orange-yellow in color, and without luster.

Identification

(1)To 10 mg of the powder add 2 ml of nitric acid solution saturated with potassium chlorate after moistening with water, dissolve, and add barium chloride test solution to produce a large amount of white precipitate. After standing, pour off the upper acid layer, add 2 ml of water, shake, and the precipitate does not dissolve.

(2)Place 0.2 g of the powder in a crucible, heat and melt, producing a white or yellowish-white flame with white smoke. After covering with a glass slide, there is white condensate, scrape off a small amount, place it in a test tube, boil with water to dissolve, filter if necessary, add a few drops of hydrogen sulfide test solution to the solution, which turns yellow, add dilute hydrochloric acid to produce a yellow flocculent precipitate, then add ammonium carbonate test solution, and the precipitate dissolves again.

Examination

Trivalent arsenic and pentavalent arsenic

Carry out the method for determination of the forms and valence states of mercury and arsenic elements <2322> in the Chinese Pharmacopoeia.

Preparation of reference solution

Accurately weigh appropriate amounts of standard reference solutions of arsenite and arsenate, dissolve in water to make a mixed solution containing 2 μg of each per ml (calculated as arsenic).

Preparation of standard curve solution

Accurately pipette appropriate amounts of the reference solution into a 1 ml volumetric flask, and prepare a series of solutions containing 5 ng, 20 ng, 50 ng, 100 ng, 200 ng, 500 ng, and 1000 ng of each valence state of arsenic (calculated as arsenic) per ml by adding 0.02 mol/L disodium ethylenediaminetetraacetate solution, respectively.

Preparation of test solution

Weigh about 30 mg of the powder (passed through a No. 5 sieve) of the test substance accurately, place it in a 250 ml plastic volumetric flask, add about 200 ml of artificial intestinal fluid, shake well, treat it with ultrasound in a 37°C water bath (power 300 W, frequency 45 kHz) for 2 hours (shake well every 15 minutes), cool, dilute with artificial intestinal fluid to the mark, shake well, take an appropriate amount and place it in a 50 ml plastic centrifuge tube, let it stand for 20-24 hours, gently blow away the surface solution with an ear syringe, and take about 15 ml of the middle solution (avoid bringing in particles when suctioning), filter through a microporous membrane (10 μm), accurately pipette 5 ml of the filtrate, place it in a 50 ml plastic volumetric flask, dilute with 0.02 mol/L disodium ethylenediaminetetraacetate solution to the mark, shake well, and obtain the test solution. Prepare the reagent blank solution in the same manner.

Determination method

Accurately pipette 20 μl of each of the standard curve solution and the test solution, inject into the liquid chromatography-inductively coupled plasma mass spectrometry system, and determine. Use the peak area of different valence states of arsenic obtained from the standard curve solution as the ordinate and the corresponding concentration as the abscissa to draw the standard curve and calculate the content of valence states of arsenic in the test solution.

The total amount of trivalent arsenic and pentavalent arsenic in the product shall not exceed 7.0% (calculated as arsenic, As).

Assay

Weigh about 0.1 g of the powder of the test substance accurately, place it in a conical flask, add 1 g of potassium sulfate, 2 g of ammonium sulfate, and 8 ml of sulfuric acid, heat directly with a flame until the solution is clear, cool, slowly add 50 ml of water, heat to a slight boil for 3-5 minutes, cool, add 2 drops of phenolphthalein indicator, titrate with sodium hydroxide solution (40→100) to a faint red color, cool, titrate with 0.25 mol/L sulfuric acid solution to colorless, add 5 g of sodium bicarbonate, shake well, titrate with iodine titration solution (0.05 mol/L) until near the end point, add 2 ml of starch indicator solution, and titrate to a purple-blue color. Each 1 ml of iodine titration solution (0.05 mol/L) is equivalent to 5.348 mg of arsenic disulfide (As2S2).

The content of arsenic in the product shall not be less than 90.0% (calculated as arsenic disulfide, As2S2).

Prepared slices

Realgar powder

Processing

Take the realgar according to the water flying method (method 0213) , and then dried.

Description

This product is orange-yellow or orange-red very fine powder, easy to stick to the hand, the gas is special.

Identification

Same as the crude drug.

Examination

Same as the crude drug.

Assay

Same as the crude drug.

Property

Pungent and warm; toxic.

Flavor

Pungent.

Meridian tropism

Liver and large intestine meridians.

Actions

To detoxify and kill insects, dry dampness and resolve phlegm, and interrupt malaria.

Indications

Used for abscesses, boils, snake and insect bites, abdominal pain due to worm accumulation, epilepsy, and malaria.

Dosage

0.05-0.1 g；For external use, apply an appropriate amount.

Administration

For oral administration in pills or powders；for external use to fumigate or smear the affected area.

Precautions

Internal use should be cautious; long-term use is prohibited; pregnant women should not use it.

Storage

Store in a dry place, tightly sealed.

雄黄

Text reference: Chinese Pharmacopoeia (2015 Edition)

Overview

Realgar is a mineral of sulfides of realgar group, containing mainly arsenic disulfide (As2S2). The drug is collected, removed from foreign matter.

Description

Aggregates of lumpy or granulous masses, irregular, dark red or orange-red streak, pale orange-red; crystal surface showing diamond-like lustre. Texture fragile, easily broken, fracture with resin-like lustre. Odour, slightly stinking characteristic taste, weak.

Identification

To 10 mg of the powder, moisten with water, add 2 ml of nitric acid solution saturated with potassium chlorate to dissolve, add barium chloride TS, a large quantity of white precipitate is produced. Allow to stand, decant the supernatant, add 2 ml of water to the precipitate and shake, it is not dissolved.

Melt 0.2 g of the powder in a crucible, a white or yellowish-white flame is produced with white heavy fume. Cover the crucible with a piece of glass, a white condensate is produced. Dissolve a small quantity of the condensate in water by boiling in a test tube, filter if necessary, then add several drops of hydrogen sulfide TS; a yellow colour is produced, and a yellow flocculent precipitate is produced on adding dilute hydrochloric acid TS, then add ammonium carbonate TS, the precipitate is dissolved.

Examination

Arsenic trioxide

To 0.94 g of the fine powder, accurately weighed, add 20 ml of dilute hydrochloric acid TS, stir constantly for 30 minutes, filter, wash the residue with two 10-ml quantities of dilute hydrochloric acid TS by stirring for 10 minutes. Combine the filtrate and washings into a 500 ml volumetric flask, add water to volume, mix well. Measure accurately 10 ml into a 100 ml volumetric flask, dilute with water to volume, mix well. To 2 ml, accurately measured, add 5 ml of hydrochloric acid and 21 ml of water. Carry out the limit test for arsenic<0822, method>,any stain produced is not more intense than that produced by standard arsenic solution.

Assay

Heat about 0.1 g of the powder, accurately weighed, in a 250 ml conical flask with 1 g of potassium sulfate, 2 g of ammonium sulfate and 8 ml of sulfuric acid until the solution becomes clear. Allow to cool, add 50 ml of water slowly, heat to boil gently for 3-5 minutes and allow to cool. Add 2 drops of phenolphthalein IS, neutralize with sodium hydroxide solution (40→100) until it becomes pale red, allow to cool, neutralize with sulfuric acid solution (0.25 mol/L) to colourless. Add 5 g of sodium bicarbonate, shake well, titrate with iodine (0.1 mol/L) VS, towards the end of titration, add 2 ml of starch IS, continue to titrate until a purplish-blue colour is produced. Each ml of iodine (0.1 mol/L) VS is equivalent to 5.348 mg of arsenic disulfide (As2S2).

It contains not less than 90.0 per cent of arsenic, calculated as arsenic disulfide (As2S2).

Prepared slices

Realgar

Processing

Levigate Realgar as described under the method for levigating <0213> and dry in the shade.

Carry out the above limit test for arsenic trioxide, the result complies with the requirements.

Property

Warm; pungent; toxic.

Flavor

Pungent.

Meridian tropism

Liver and large intestine meridians.

Actions

To remove toxin, kill worms, dry dampness, dispel phlegm, and interrupt malaria.

Indications

Swelling abscess, deep rooted boil and sore, bites of insect, worm or snake, abdominal pain caused by worm accumulation, fright epilepsy, and malaria.

Dosage

0.05-0.1 g.

Administration

Used in pills or powder.

Appropriate amount for topical application, fume to pars affecta.

Precautions and Warnings

Used cautiously for oral administration. Avoid long-term administration. Contraindicated for pregnant woman.

Storage

Preserve in a tightly closed container, and store in a dry place.