JPS5936605B2 - Production method of "Shiya" laxative - Google Patents

Description

[Detailed description of the invention] The present invention relates to a method for producing laxatives.

More specifically, the present invention relates to a method for producing a laxative, which comprises collecting sennosides as lead salts from a solution containing sennosides, and then removing lead from the lead salts as lead sulfate or lead halide. Traditionally, senna leaves and senna leaves have been used as herbal medicines with laxative effects, and their active ingredients include sennosides (sennosides A, B, , C, D, , E, and F) and oxyanthraquinones such as glucosylrein. Although derivatives are known, lagoonal purposes were usually achieved in ancient times or by means such as taking powdered senna leaves or extracts extracted with water, hydroalcohol, etc. However, since the laxative is a natural product, its quality is not always consistent, which often causes inconvenience during treatment. There is also the disadvantage that the dosage must be increased. A long time ago, there have been several attempts to solve the above-mentioned disadvantages by purifying and concentrating the active ingredients of senna leaves.

However, due to the variety of chemical characteristics of the active ingredients, there are cases where only a part of the active ingredients can be extracted, or impurities cannot be removed sufficiently, and therefore high-potency laxatives are used. In other words, they were not always able to fully achieve their goals. The main object of the present invention is to provide a high-potency laxative containing not only sennosides as the main active ingredient but also oxyanthraquinone derivatives by using senna leaves in a very simple manner. The solutions containing sennosides used in the present invention are usually obtained by extracting ancient or senna leaves. Extraction is usually carried out by crushing the senna leaves or by using 5 to 10 times their weight of water or a water-containing solvent. The solvent that can be used in combination with water is a hydrophilic organic solvent, such as lower alcohols such as methanol and ethanol, ethers such as tetrahydrofuran and dioxane, and ketones such as acetone and methyl ethyl ketone. Preferably, the extraction is carried out at a temperature below 60°C.

The extraction time cannot be specified as it depends on the solvent used and the degree of extraction, but it is taken as an indicator until a darkly colored extract can no longer be obtained from the extraction residue. Since the extract has been further concentrated if desired, it may be redissolved in a solvent such as, for example, aqueous methanol. The solution containing sennosides thus obtained contains impurities such as oxyanthraquinone derivatives and ineffective components in addition to sennosides. When a weak acid salt of lead is applied to a solution containing such sennosides, lead salts of sennosides are generated.

As the weak acid salt of lead, one with relatively high water solubility is preferable, and lead acetate is most suitable. It is convenient to use the weak acid salt of lead as an aqueous solution. Although the amount of weak lead acid salt to be used cannot be determined unconditionally, it is usually about 1/3 to 1/10 (by weight) of dried rhubarb or senna leaves used as raw materials. In this way, a precipitate containing lead salts of oxyanthraquinone derivatives and some impurity lead salts in addition to lead salts of sennosides is formed, and this precipitate is collected by means such as P filtration. The precipitate thus obtained is subjected to a deleading step.

Deleading is usually carried out by treating the precipitate with alkali metal, alkaline earth metal or ammonia sulphates or halides. The precipitate is added to an aqueous solution of an alkali metal, alkaline earth metal, or ammonia sulfate or halide in an amount equivalent to the amount of lead commonly used, and the mixture is thoroughly stirred to sufficiently generate lead sulfate or lead halide. The reaction mixture can be used as is or in about 1 to 2 times the amount of water in the reaction mixture (
After adding a hydrophilic organic solvent such as alcohol (for example, methanol) in an amount of about
By adding twice the amount of a water-containing solvent (usually a water-containing alcohol such as water-containing methanol) and stirring well, the soluble portion is removed and concentrated to produce a high-potency laxative in the form of a brown powder. You can go around. The water in the hydrous alcohol is desirably 1/4 (weight) or less of the alcohol. In addition, in the process of obtaining the soluble portion, it is also permissible to bias the temperature up to 50° C. in order to promote dissolution of the target object.

Impurities and lead sulfate or lead halides are removed as insoluble materials. The sennoside and carboxyl group-containing oxyanthraquinone derivatives contained in the laxatives obtained by this process are usually salts with alkali metals, alkaline earth metals, or ammonia, but if desired, they can be converted into salts by known means. Therefore, it may be converted into the free acid or other salts. The laxative produced according to the present invention contains sennosides and oxyanthraquinone derivatives and is prepared by the method of Fujimura et al. [Japan Pharmacological Journal Dan 1634 (1969).
)], the lagoonal activity in mice was 50%.
It shows an effective rate (ED5O) of about 40~/Kg, and when administered orally to the human body as a laxative, it is 30~5/Kg per day for adults.
You can reach your goal in 01if7.

The yield varies depending on the raw material, but for example, it is 6 to 11% from rhubarb with a mouse lagoonal activity of 185 my/Kg, and about 2% from senna leaves, which also has a 311-/Kg. Detailed procedures will be shown below with reference to Examples, but the Examples are not intended to limit the present invention. Example 1 Powdered rhubarb (ED, Ol85~/Kg) 700 at 100V
A 50% methanol aqueous solution of m1 was added, and the mixture was extracted at 50°C for 2 hours, and then filtered through P.

25y lead acetate [Pb(0C0CH3)2.3
After adding 200 ml of an aqueous solution containing [H20] and leaving it for 3 hours, the precipitate deposited was collected and thoroughly washed with a 50% methanol aqueous solution. Add 10% salt (A) aqueous solution 2 to the precipitate.
After adding 0.00g and stirring vigorously, 200ml of methanol was added and insoluble matter was removed.

After concentrating the soluble portion under reduced pressure at 50°C, the residue was reduced to 90%.
Extraction was performed with 400 ml of methanol aqueous solution to remove insoluble matter again. When the soluble portion was concentrated, an ocher or brown powder was obtained. This product contains sennoside A and other sennosides as well as oxyanthraquinone derivatives such as glucosylrein. The salt (A) used, the yield from the raw materials, and the lagoonal activity in mice are shown in the table below. Example 2 Powdered rhubarb (ED5Ol85~/Kg) 700 to 100V
After adding 1 m of water and extracting at 50°C for 3 hours, the mixture was filtered, the residue was washed with water at 50°C, and then filtered again.

The extract and washing liquid were combined and 250 liters of a 10% aqueous lead acetate solution was added to obtain a precipitate. 200 ml of 10% potassium sulfate aqueous solution was added to the precipitate, stirred well, and then concentrated to dryness. 400 ml of 80% methanol aqueous solution was added to the residue and extracted at 50°C. After removing insoluble matter, the extract was concentrated to obtain active fraction 6.3f7. ED, O4l. 2~/
Kg Example 3 Powdered senna leaf (ED5O3ll~/Kg) 5 to 1007
A 0% aqueous methanol solution 1,e was added and extracted at 50°C for 2 hours, followed by filtration.

▲After adding 350ml of 10% lead acetate aqueous solution to the solution,
The mixture was left to stand for a while, and the precipitate deposited was filtered off. 10 to the precipitate
After adding 100 ml of % sodium sulfate aqueous solution and stirring well, 100 ml of methanol was added to remove insoluble materials. After concentrating the soluble portion at 50°C, 300 ml of 90% aqueous methanol solution was added to obtain 1.7f7 of brown powder. ED
5O value: 48.2W9/l<g Sea bream 4 100ml of a 10% potassium sulfate aqueous solution was added to the lead salt obtained in the same manner as in Example 3, stirred well, and then concentrated at 50°C.

Claims (1)

[Claims] 1. A method for producing a laxative, which comprises collecting sennosides as lead salts from a solution containing sennosides, and then removing lead from the lead salts as lead sulfate or lead halide.