CN1709355A - Oldenlandia diffusa roxb injection agent, and its preparing method and quality control method - Google Patents

Abstract

The present invention relates to a hedyotis injection. It is a hedyotis powder injection or freeze-dried powder injection whose main component is hedyotis extract. Said invention also provides the concrete steps of its preparation method, and its quality control method adopts a content assaying method, so that the controllability and stability of said product quality can be greatly raised.

Description

A kind of oldenlandia diffusa roxb injection agent and preparation method thereof and method of quality control

Technical field:

This invention relates to a kind of Chinese medicine and preparation method thereof and method of quality control, relates in particular to injection Herba Hedyotidis Diffusae grass meal pin or freeze-dried powder and preparation method thereof and method of quality control.

Background technology:

Powder pin or freeze-dried powder, change dosage form and manage as new drug research according to the relevant laws and regulations of China's drug control as a kind of pharmaceutical dosage form.This product has BAIHUASHESHECAO ZHUSHEYE now, has listed the national drug ministry standard in.

The technology features of existing BAIHUASHESHECAO ZHUSHEYE is with the Herba Hedyotidis Diffusae in the prescription, according to percolation, makes solvent with ethanol, dipping, percolation, concentrate the liquid of filtering, regulate pH value, cold preservation filters, and regulates pH value, leave standstill, filter, transfer PH, add ethanol to neutral, cold preservation filters, and filtrate decompression concentrates, and adds water, regulate pH value, add an amount of Polysorbate and sodium sulfite, fully stir evenly, filter, add the injection water to ormal weight, embedding, sterilization, promptly.

Existing BAIHUASHESHECAO ZHUSHEYE is subject to factors of affecting such as making, storage, and the difficult control of quality influences clinical therapeutic efficacy.

Summary of the invention:

The purpose of this invention is to provide a kind of oldenlandia diffusa roxb injection agent and preparation method thereof and method of quality control, overcome the above-mentioned disadvantage of prior art BAIHUASHESHECAO ZHUSHEYE, improve the quality and the curative effect of product, satisfy the needs of medical treatment better.

Technical solution of the present invention is a kind of oldenlandia diffusa roxb injection agent, and it is that main component is injection Herba Hedyotidis Diffusae grass meal pin or the freeze-dried powder of Herba Hedyotidis Diffusae.

The preparation method of injection Herba Hedyotidis Diffusae grass meal pin or freeze-dried powder: get Herba Hedyotidis Diffusae, be ground into coarse powder, according to percolation, make solvent with 70-90% ethanol, flooded 20-30 hour, slowly percolation, concentrate the liquid of filtering, regulate pH value with lime cream, cold preservation, filter, filtrate is regulated pH value with the 25-75% sulfuric acid solution, leaves standstill, filter, filtrate reuse 20-60% sodium hydroxide solution is regulated pH value to neutral, adds ethanol, cold preservation, filter, filtrate decompression concentrates, and adds water, regulate pH value with the 20-60% sodium hydroxide solution, after adding an amount of adjuvant, stirring is dissolved it fully, adds charcoal treatment again, filter, must not have the clear and bright solution of thermal source, dry must not have the thermal source powder, will not have the packing of thermal source powder, gland promptly gets injection Herba Hedyotidis Diffusae grass meal pin; Maybe will there be the clear and bright solution of thermal source, packing, lyophilization, gland promptly gets injection Herba Hedyotidis Diffusae freeze-dried powder.

Its adjuvant is mixture or other proper auxiliary materials of following one or more: Polysorbate, disodiumedetate, citric acid (sodium), sodium sulfite, sodium sulfite, sodium pyrosulfite, sodium thiosulfate, vitamin C, nitrogen, mannitol, dextran, lactose or glucose.

The method of quality control of injection Herba Hedyotidis Diffusae grass meal pin or freeze-dried powder is: assay adopts high effective liquid chromatography for measuring, octadecylsilane chemically bonded silica is a filler, and mobile phase is methanol-10-30mmol/LNH4Ac (pH3.5) (20-40: 50-60); The detection wavelength is 250-350nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 5700; It is an amount of that the preparation of reference substance solution, precision take by weighing the coumaric acid reference substance, adds methanol and make the solution that every 1ml contains 70-90ug, promptly;

This product 1-4g is measured in the preparation of need testing solution, precision, uses dissolve with methanol, puts in the 10ml measuring bottle, adds methanol to scale, shakes up, and filters, and gets subsequent filtrate as need testing solution;

Algoscopy, accurate respectively need testing solution and each 20 μ l of reference substance solution of drawing inject chromatograph of liquid, measure.

Specific embodiments:

The present invention further specifies as follows in conjunction with specific embodiments:

A kind of oldenlandia diffusa roxb injection agent, it is that main component is injection Herba Hedyotidis Diffusae grass meal pin or the freeze-dried powder of Herba Hedyotidis Diffusae.

Chinese medicine preparation of the present invention is mainly used in warm respiratory tract infection of accumulateing due to the poison, tonsillitis, and pneumonia, cholecystitis, appendicitis, carbuncle furuncle abscess and use postoperative infection also can be used for assistant treating cancer.

Embodiment one:

Get Herba Hedyotidis Diffusae 1000g, be ground into coarse powder, according to the percolation (pharmacopeia appendix IO) under fluid extract and the extractum item, make solvent with 80% ethanol, flooded 24 hours, slowly percolation, the liquid of filtering is concentrated into about 250ml, regulates pH value to 12, cold preservation 12 hours with lime cream, filter, it is 3 that filtrate is regulated pH value with 50% sulfuric acid solution, leaves standstill 12 hours, filter, filtrate reuse 40% sodium hydroxide solution is regulated pH value to neutral, adds ethanol 2000ml, cold preservation 24 hours, filter, filtrate decompression is concentrated into 250ml, adds water to 500ml, regulating pH value with 40% sodium hydroxide solution is 6.5～7.0, add the injection water, cooling is left standstill, and makes 1000ml altogether, add active carbon, stir, boiled cold filtration 10 minutes, add an amount of water for injection, must not have the clear and bright solution of thermal source, dry must not have the thermal source powder, will not have the packing of thermal source powder, gland promptly gets injection Herba Hedyotidis Diffusae grass meal pin; Maybe will there be the clear and bright solution of thermal source, packing, lyophilization, gland promptly gets injection Herba Hedyotidis Diffusae freeze-dried powder.

Embodiment two:

Get Herba Hedyotidis Diffusae 1000g, be ground into coarse powder, according to the percolation (pharmacopeia appendix IO) under fluid extract and the extractum item, make solvent with 80% ethanol, flooded 24 hours, slowly percolation, the liquid of filtering is concentrated into about 250ml, regulates pH value to 12, cold preservation 12 hours with lime cream, filter, it is 3 that filtrate is regulated pH value with 50% sulfuric acid solution, leaves standstill 12 hours, filter, filtrate reuse 40% sodium hydroxide solution is regulated pH value to neutral, adds ethanol 2000ml, cold preservation 24 hours, filter, filtrate decompression is concentrated into 250ml, adds water to 500ml, and regulating pH value with 40% sodium hydroxide solution is 6.5～7.0, add the injection water, cooling is left standstill, and makes 1000ml altogether, adds 0.1% sodium sulfite or sodium pyrosulfite stabilizing agent or its mixture, mannitol with 3% is as proppant, stirring is dissolved it fully, add 0.05% charcoal treatment again, filter, must not have the clear and bright solution of thermal source, dry must not have the thermal source powder, to not have the packing of thermal source powder, gland promptly gets injection Herba Hedyotidis Diffusae grass meal pin; Maybe will there be the clear and bright solution of thermal source, packing, lyophilization, gland promptly gets injection Herba Hedyotidis Diffusae freeze-dried powder.

Embodiment three:

Get Herba Hedyotidis Diffusae 1000g, be ground into coarse powder, according to the percolation under fluid extract and the extractum item (pharmacopeia appendix IO), make solvent with 80% ethanol, flooded 24 hours, percolation slowly, the liquid of filtering is concentrated into about 250ml, regulates pH value to 12 with lime cream, cold preservation 12 hours, filter, it is 3 that filtrate is regulated pH value with 50% sulfuric acid solution, leaves standstill 12 hours, filter, filtrate reuse 40% sodium hydroxide solution is regulated pH value to neutral, adds ethanol 2000ml, cold preservation 24 hours, filter, filtrate decompression is concentrated into 250ml, adds water to 500ml, and regulating pH value with 40% sodium hydroxide solution is 6.5～7.0, add the 10g polyoxyethylene sorbitan monoleate, fully stir evenly, filter, add the injection water, cooling is left standstill, make 1000ml altogether, add 0.05% stabilizing agent sodium sulfite or vitamin C or its mixture, or the inflated with nitrogen used as stabilizers, add 3% dextran again as proppant, stirring is dissolved it fully, add 0.05% charcoal treatment again, filter, must not have the clear and bright solution of thermal source, dry must not have the thermal source powder, to not have the packing of thermal source powder, gland promptly gets injection Herba Hedyotidis Diffusae grass meal pin; Maybe will there be the clear and bright solution of thermal source, packing, lyophilization, gland promptly gets injection Herba Hedyotidis Diffusae freeze-dried powder.

Embodiment four:

Get Herba Hedyotidis Diffusae 1000g, be ground into coarse powder, according to the percolation under fluid extract and the extractum item (pharmacopeia appendix IO), make solvent with 80% ethanol, flooded 24 hours, percolation slowly, the liquid of filtering is concentrated into about 250ml, regulates pH value to 12, cold preservation 12 hours with lime cream, filter, it is 3 that filtrate is regulated pH value with 50% sulfuric acid solution, leaves standstill 12 hours, filters, filtrate reuse 40% sodium hydroxide solution is regulated pH value to neutral, add ethanol 2000ml, cold preservation 24 hours filters, filtrate decompression is concentrated into 250ml, add water to 500ml, regulating pH value with 40% sodium hydroxide solution is 6.5～7.0, adds the 10g polyoxyethylene sorbitan monoleate, fully stir evenly, filter, add the injection water, cooling is left standstill, make 1000ml altogether, the sodium thiosulfate used as stabilizers of adding 0.02% and 5% lactose or glucose or its mixture are done proppant, stir it is dissolved fully, add 0.01% charcoal treatment again, filter, must not have the clear and bright solution of thermal source, dry must not have the thermal source powder, will not have the packing of thermal source powder, gland promptly gets injection Herba Hedyotidis Diffusae grass meal pin; Maybe will there be the clear and bright solution of thermal source, packing, lyophilization, gland promptly gets injection Herba Hedyotidis Diffusae freeze-dried powder.

The method of quality control of a kind of oldenlandia diffusa roxb injection agent injection Herba Hedyotidis Diffusae grass meal pin or freeze-dried powder is:

Assay, according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, methanol-20mmol/L NH4Ac (pH3.5) (33: 67) is a mobile phase; The detection wavelength is 308nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 5700; It is an amount of that the preparation of reference substance solution, precision take by weighing the coumaric acid reference substance, adds methanol and make the solution that every 1ml contains 80ug, promptly;

This product 2g is measured in the preparation of need testing solution, precision, uses dissolve with methanol, puts in the 10ml measuring bottle, adds methanol to scale, shakes up, and filters, and gets subsequent filtrate as need testing solution;

Algoscopy, accurate respectively need testing solution and each 20 μ l of reference substance solution of drawing inject chromatograph of liquid, measure.

Advantage of the present invention is:

Improved controllability and the stability of product quality, guaranteed the safe, effective of clinical application, be conducive to produce The storage of product.

Claims (4)

1, a kind of oldenlandia diffusa roxb injection agent is characterized in that it is that main component is injection Herba Hedyotidis Diffusae grass meal pin or the freeze-dried powder of Herba Hedyotidis Diffusae.

2, a kind of preparation method of oldenlandia diffusa roxb injection agent, it is the preparation method of injection Herba Hedyotidis Diffusae grass meal pin or freeze-dried powder, it is characterized in that:

(1) medical ingredient is a Herba Hedyotidis Diffusae;

(2) get Herba Hedyotidis Diffusae, be ground into coarse powder, according to percolation, make solvent with 70-90% ethanol, flooded 20-30 hour, slowly percolation, concentrate the liquid of filtering, regulate pH value with lime cream, cold preservation, filter, filtrate is regulated pH value with the 25-75% sulfuric acid solution, leaves standstill, filter, filtrate reuse 20-60% sodium hydroxide solution is regulated pH value to neutral, adds ethanol, cold preservation, filter, filtrate decompression concentrates, and adds water, regulate pH value with the 20-60% sodium hydroxide solution, after adding an amount of adjuvant, stirring is dissolved it fully, adds charcoal treatment again, filter, must not have the clear and bright solution of thermal source, dry must not have the thermal source powder, will not have the packing of thermal source powder, gland promptly gets injection Herba Hedyotidis Diffusae grass meal pin; Maybe will there be the clear and bright solution of thermal source, packing, lyophilization, gland promptly gets injection Herba Hedyotidis Diffusae freeze-dried powder.

3, the preparation method of a kind of oldenlandia diffusa roxb injection agent according to claim 2 is characterized in that its said adjuvant is mixture or other proper auxiliary materials of following one or more: Polysorbate, disodiumedetate, citric acid (sodium), sodium sulfite, sodium sulfite, sodium pyrosulfite, sodium thiosulfate, vitamin C, nitrogen, mannitol, dextran, lactose or glucose.

4, a kind of method of quality control of oldenlandia diffusa roxb injection agent, it is the method for quality control of injection Herba Hedyotidis Diffusae grass meal pin or freeze-dried powder, it is characterized in that: assay adopts high effective liquid chromatography for measuring, octadecylsilane chemically bonded silica is a filler, methanol-10～30mmol/L NH4Ac (PH3.5) (20～40: 50～60) be mobile phase; The detection wavelength is 250～350nm; Number of theoretical plate calculates by the coumaric acid peak should be not less than 2000; It is an amount of that the preparation of reference substance solution, precision take by weighing the coumaric acid reference substance, adds methanol and make the solution that every 1ml contains 70-90ug, promptly;

This product 1-4g is measured in the preparation of need testing solution, precision, uses dissolve with methanol, puts in the 10ml measuring bottle, adds methanol to scale, shakes up, and filters, and gets subsequent filtrate as need testing solution;

Algoscopy, accurate respectively need testing solution and each 20 μ l of reference substance solution of drawing inject chromatograph of liquid, measure.