Quality control method for quick-acting antidiarrheal capsule

Abstract

The invention discloses a quality control method of Suxiaozhixie Capsule, which comprises the following steps: identifying the capsule, detecting content according to high performance liquid chromatography: A chromatographic condition and system qualification test, B preparing contrast solution, C preparing testing solution for assay, and D precisely sucking 10 mu l contrast solution and testing solution for assay respectively, injecting into liquid chromatograph, detecting, wherein, labelled amount of berberine hydrochloride in the product is 90-110%.The invention can better control the quality of the capsule, guarantee safety for administration, guide production with rational and strict process control.

Description

technical field

[0001] The invention belongs to the field of quality control of traditional Chinese medicine preparations, in particular to a quality control method for Suxiao Zhixie Capsules. Background technique

[0002] Suxiao Zhixie Capsules are composed of berberine hydrochloride and boxing ginseng, which have the functions of clearing heat and dampness, astringent and antidiarrheal; it is used for red dysentery, heat diarrhea, enteritis, etc. The Suxiao Zhixie Capsules described in the drug standards of the Ministry of Health of the People's Republic of China only provides a qualitative detection method for berberine hydrochloride, and lacks the identification and determination methods of other main medicinal flavors of the drug, which cannot effectively control the product quality. Contents of the invention

[0003] The object of the present invention is to overcome the above-mentioned shortcoming and provide a kind of quality control method that can effectively ide...

Examples

Embodiment 1

[0015] (1) Identification of Suxiao Zhixie Capsules: Take about 0.1g of the contents of the finished capsule, add 2ml of dilute hydrochloric acid, stir to dissolve, add a little bleaching powder, and it will appear dark cherry red;

[0016] (2) Determination of content according to high performance liquid chromatography:

[0017] A. Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler; 0.05mol / L potassium dihydrogen phosphate-acetonitrile-triethylamine (60:40:0.1) as mobile phase; detection wavelength 346nm. The number of theoretical plates should not be less than 3000 based on the berberine hydrochloride peak;

[0018] B. Preparation of reference substance solution: accurately weigh an appropriate amount of berberine hydrochloride reference substance, add methanol to make a solution containing 0.4mg per 1ml, to obtain final product;

[0019] C. Preparation of the test solution: take about 100 mg of the finished capsule cont...

Embodiment 2

[0022] (1) Identification of quick-acting antidiarrheal capsules: take 0.5 g of the contents of the finished capsule, add 5 ml of methanol, stir to dissolve, filter, and the filtrate is used as the test solution. Take another berberine hydrochloride reference substance, add methanol to make a solution containing 0.5mg per 1ml, as the reference substance solution. According to thin-layer chromatography, draw 2 μl of each of the above two solutions, and spot them on the same silica gel G thin-layer plate with 0.5% sodium carboxymethylcellulose as a binder, and mix with n-butanol-glacial acetic acid-water ( 7:1:2) as developer, develop, take out, dry, and inspect under ultraviolet light (365nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the reference product, fluorescent spots of the same color appear;

[0023] (2) Determination of content according to high performance liquid chromatography:

[0024] A. Chromatographic conditi...

Embodiment 3

[0029] (1) Identification of quick-acting antidiarrheal capsules: take 1 g of the finished capsule content, add 20 ml of 95% ethanol and ultrasonically dry it for 30 minutes, filter, evaporate the filtrate to dryness, add 5 ml of ethyl acetate to the residue and ultrasonically dissolve it, filter, and evaporate the filtrate to dryness , add 1ml of ethyl acetate to the residue to dissolve, and use it as the test solution; take 0.5g of ginseng reference medicinal material, add 20ml of 95% ethanol to ultrasonic for 30 minutes, filter, evaporate the filtrate to dryness, add 1ml of ethyl acetate to the residue to dissolve, As a contrast medicinal material solution; take 15 μl each of the above-mentioned need testing solution and the contrast medicinal material solution, according to thin-layer chromatography, respectively spot on the same silica gel G thin-layer plate, use chloroform: methanol (19: 1) as developing agent, develop, Take it out, dry it in the air, spray it with 5% eth...

technical field

[0001] The invention belongs to the field of quality control of traditional Chinese medicine preparations, in particular to a quality control method for Suxiao Zhixie Capsules. Background technique

[0002] Suxiao Zhixie Capsules are composed of berberine hydrochloride and boxing ginseng, which have the functions of clearing heat and dampness, astringent and antidiarrheal; it is used for red dysentery, heat diarrhea, enteritis, etc. The Suxiao Zhixie Capsules described in the drug standards of the Ministry of Health of the People's Republic of China only provides a qualitative detection method for berberine hydrochloride, and lacks the identification and determination methods of other main medicinal flavors of the drug, which cannot effectively control the product quality. Contents of the invention

[0003] The object of the present invention is to overcome the above-mentioned shortcoming and provide a kind of quality control method that can effectively ide...

Examples

Embodiment 1

[0015] (1) Identification of Suxiao Zhixie Capsules: Take about 0.1g of the contents of the finished capsule, add 2ml of dilute hydrochloric acid, stir to dissolve, add a little bleaching powder, and it will appear dark cherry red;

[0016] (2) Determination of content according to high performance liquid chromatography:

[0017] A. Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler; 0.05mol / L potassium dihydrogen phosphate-acetonitrile-triethylamine (60:40:0.1) as mobile phase; detection wavelength 346nm. The number of theoretical plates should not be less than 3000 based on the berberine hydrochloride peak;

[0018] B. Preparation of reference substance solution: accurately weigh an appropriate amount of berberine hydrochloride reference substance, add methanol to make a solution containing 0.4mg per 1ml, to obtain final product;

[0019] C. Preparation of the test solution: take about 100 mg of the finished capsule cont...

Embodiment 2

[0022] (1) Identification of quick-acting antidiarrheal capsules: take 0.5 g of the contents of the finished capsule, add 5 ml of methanol, stir to dissolve, filter, and the filtrate is used as the test solution. Take another berberine hydrochloride reference substance, add methanol to make a solution containing 0.5mg per 1ml, as the reference substance solution. According to thin-layer chromatography, draw 2 μl of each of the above two solutions, and spot them on the same silica gel G thin-layer plate with 0.5% sodium carboxymethylcellulose as a binder, and mix with n-butanol-glacial acetic acid-water ( 7:1:2) as developer, develop, take out, dry, and inspect under ultraviolet light (365nm). In the chromatogram of the test product, at the position corresponding to the chromatogram of the reference product, fluorescent spots of the same color appear;

[0023] (2) Determination of content according to high performance liquid chromatography:

[0024] A. Chromatographic conditi...

Embodiment 3

[0029] (1) Identification of quick-acting antidiarrheal capsules: take 1 g of the finished capsule content, add 20 ml of 95% ethanol and ultrasonically dry it for 30 minutes, filter, evaporate the filtrate to dryness, add 5 ml of ethyl acetate to the residue and ultrasonically dissolve it, filter, and evaporate the filtrate to dryness , add 1ml of ethyl acetate to the residue to dissolve, and use it as the test solution; take 0.5g of ginseng reference medicinal material, add 20ml of 95% ethanol to ultrasonic for 30 minutes, filter, evaporate the filtrate to dryness, add 1ml of ethyl acetate to the residue to dissolve, As a contrast medicinal material solution; take 15 μl each of the above-mentioned need testing solution and the contrast medicinal material solution, according to thin-layer chromatography, respectively spot on the same silica gel G thin-layer plate, use chloroform: methanol (19: 1) as developing agent, develop, Take it out, dry it in the air, spray it with 5% eth...