阅读说明：本技术 一种紫草配方颗粒的制备方法及其质量标准 (Preparation method and quality standard of lithospermum formula granules ) 是由 上官同强 于秀玲 韩风雨 艾林 于 2019-11-27 设计创作，主要内容包括：本发明公开了一种紫草配方颗粒的制备方法及其质量标准,该配方以紫草饮片为原料,经水提、干燥等流程制得紫草配方颗粒,并通过试验确定了紫草配方颗粒的薄层鉴别方法,制定了紫草配方颗粒的质量标准,为保证紫草配方颗粒质量达到稳定、可控、高效及安全提供数据支撑。(The invention discloses a preparation method and quality standard of lithospermum formula granules, the formula takes lithospermum decoction pieces as raw materials, the lithospermum formula granules are prepared by the processes of water extraction, drying and the like, the thin-layer identification method of the lithospermum formula granules is determined through experiments, the quality standard of the lithospermum formula granules is formulated, and data support is provided for ensuring that the quality of the lithospermum formula granules achieves stability, controllability, high efficiency and safety.)

1. A preparation method and quality standard of radix Arnebiae granule comprises the following steps: taking 10000g of lithospermum decoction pieces, adding water for decocting twice, filtering, concentrating the filtrate into clear paste, adding a proper amount of auxiliary materials, drying, adding the auxiliary materials, uniformly mixing, preparing into 1000g of granules, and subpackaging to obtain the lithospermum decoction pieces, wherein each 1g of the granules in the formula is equivalent to 10.0g of the decoction pieces;

the quality standard of the formula particle comprises character indexes, thin-layer chromatography identification indexes, inspection indexes and extract indexes, wherein the indexes are as follows:

(1) the characteristics are as follows: the product is brown to black brown granules; special smell, slightly bitter taste;

(2) and (3) identification:

grinding 2g of the product, adding 30ml of ethanol, heating and refluxing for 1 hour, filtering, evaporating the filtrate to dryness, and dissolving the residue in 2ml of methanol to obtain a sample solution; adding water 30ml into 2.5g radix Arnebiae control medicinal material, filtering, evaporating filtrate, and adding ethanol 30ml into residue to obtain control medicinal material solution; performing thin layer chromatography (0502 of the four ministry of the national pharmacopoeia 2015), collecting 10 μ l of each of the two solutions, developing with cyclohexane-toluene-ethyl acetate-formic acid (5: 0.5: 0.1) as developing agent, taking out, air drying, spraying 10% potassium hydroxide methanol solution, and displaying fluorescent spots of the same color in the chromatogram of the test solution at the position corresponding to the chromatogram of the control solution;

(3) examination of

Meets the related regulations under the item of the granules (0104 in the four ministry of communications in 2015 pharmacopoeia of China;

(4) extract of plant

The product is ground into fine powder, about 2g of the powder is precisely weighed, 100ml of ethanol is precisely added, and the content of the powder is not less than 5.0% as measured by hot dipping method under alcohol-soluble extract measuring method (2201 in the fourth pharmacopoeia 2015).

Technical Field

The invention relates to a preparation method and a quality standard of a traditional Chinese medicine formula granule, in particular to a preparation method and a quality standard of a lithospermum formula granule.

Background

Dried roots of Arnebia euchroma (Royle) johnst, Arnebia euchroma, or Arnebia gutta, Bunge, were recorded in the book Shennong Ben Cao Jing and the book Ben Cao Luns of physicians of different generations. Radix Arnebiae is cold in nature, sweet and salty in flavor, and enters heart and liver meridians, and has effects of stopping bleeding and cooling blood. Can be used for treating diseases such as blood heat and toxic materials, macula purple black, measles without adequate eruption, fever macula, eczema, hematuria, bloody stranguria, bloody dysentery, constipation due to heat accumulation, pyocutaneous disease, erysipelas, burn, malignant boil, and tinea.

The traditional Chinese medicine formula particle is prepared by taking traditional Chinese medicine decoction pieces as raw materials, extracting, concentrating, separating, drying, granulating and packaging by modern pharmaceutical technology. Compared with the traditional decoction pieces, the traditional Chinese medicine formula granule meets the requirement of the modern management of a traditional Chinese medicine pharmacy in a hospital, and has the advantages of small volume, light weight, convenient carrying, convenient taking and the like. The preparation principle of the traditional Chinese medicine formula particle is 'deformation without denaturation', namely the appearance of the medicine is changed, and the properties, the medicine property and the components are not changed. At present, the quality standard of the traditional Chinese medicine formula granule is not perfect, no unified national standard exists, and the internal control standard of each enterprise is established and executed.

The invention aims to provide a preparation method and a quality standard of lithospermum formula granules, and provides a certain data support for industrialized production of lithospermum formula granules by determining the quality standard and a detection method thereof.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a preparation method and a quality standard of lithospermum formula granules, and the aim of the invention is realized by the following technical scheme:

the preparation method comprises decocting 10000g of radix Arnebiae decoction pieces in water twice, filtering, concentrating the filtrate to obtain fluid extract, adding appropriate amount of adjuvant, drying, adding adjuvant, mixing, granulating to 1000g, and packaging.

The quality standard is as follows:

1. processing: removing impurities, and cutting into thick pieces or sections.

2. The preparation method comprises the following steps: taking 10000g of lithospermum decoction pieces, adding water for decocting twice, filtering, concentrating the filtrate into clear paste, adding a proper amount of auxiliary materials, drying, adding the auxiliary materials, uniformly mixing, preparing 1000g of granules, and subpackaging to obtain the traditional Chinese medicine.

3. The characteristics are as follows: the product is brown to black brown granules; special smell, slightly bitter taste.

4. And (3) identification:

grinding 2g of the product, adding 30ml of ethanol, heating and refluxing for 1 hour, filtering, evaporating the filtrate to dryness, and dissolving the residue in 2ml of methanol to obtain a sample solution. And adding water into 2.5g of radix Arnebiae control material, adding 30ml of water, filtering, evaporating the filtrate, and adding ethanol into the residue to 30ml to obtain control solution. Performing thin layer chromatography (0502 of the four ministry of the national pharmacopoeia 2015), collecting 10 μ l of each of the two solutions, developing with cyclohexane-toluene-ethyl acetate-formic acid (5: 0.5: 0.1) as developing agent, taking out, air drying, spraying 10% potassium hydroxide methanol solution, and displaying fluorescent spots of the same color in the chromatogram of the test solution at the position corresponding to the chromatogram of the control solution.

5. Examination of

Meets the regulations of granules (0104 in the four ministerial general rules of 2015, China pharmacopoeia).

6. Extract of plant

The product is ground into fine powder, about 2g of the powder is precisely weighed, 100ml of ethanol is precisely added, and the content of the powder is not less than 5.0% as measured by hot dipping method under alcohol-soluble extract measuring method (2201 in the fourth pharmacopoeia 2015).

7. Property, flavor and meridian tropism

Sweet, slightly bitter and warm. It enters spleen, lung, heart and kidney meridians.

8. Specification of

1g of the formula particle is equivalent to 10.0g of decoction pieces.

Compared with the prior art, the invention has the following advantages and beneficial effects:

the invention defines the preparation process of the lithospermum formula granules, establishes quality standards such as lithospermum thin-layer chromatography identification and the like, and can effectively control the quality of the lithospermum formula granules, so that the quality of the lithospermum formula granules achieves stability, controllability, high efficiency and safety.

Detailed Description

The following detailed description of the embodiments of the present invention is provided for the purpose of illustration and not limitation, and should not be construed as limiting the scope of the invention.

Test example 1

Thin layer identification research of lithospermum formula granules

Referring to the method under the item of identifying Lithospermum erythrorhizon in the first edition of Chinese pharmacopoeia 2015, the obtained thin-layer chromatography spots are not clear. Through the method exploration, a text method is formulated. The concrete description is as follows: :

1. reagent and medicinal material

Lithospermum as a reference medicinal material: batch No. 121430-201504, purchased from China institute for food and drug testing;

and (3) testing the sample: batch numbers 171813001, 171813002, 171813003

Thin-layer plate: silica gel G plate. All reagents are analytically pure.

2. Chromatographic conditions

Thin-layer plate: silica gel G plate. Sample amount of spotting: 10. mu.l each.

Developing agent: cyclohexane-toluene-ethyl acetate-formic acid (5: 0.5: 0.1).

Color development and inspection: spraying 10% ethanol sulfate solution to obtain fluorescent spots with the same color.

3. Investigation of

3.1 negative interference Experimental investigation

Preparing a negative sample solution according to the method for preparing the test solution in the text standard, preparing the test solution and the control solution simultaneously, and respectively dropping the test solution and the control solution on the same thin-layer plate, wherein the result shows that spots on the corresponding positions of the thin-layer chromatography of the test solution and the control solution are clear in color development, and the negative sample has no color spots and is proved to be negative and non-interference.

3.2 method reproducibility examination

The three batches of samples are taken and checked according to the determined conditions, and the results show that the thin-layer chromatography spots of the three batches of samples are clear and have good reproducibility, so the identification method of the product is shown in the text

Test example 2

Investigation of extract of lithospermum formula particles

The gromwell formula particles were examined according to the hot dipping method under 2201 extract determination item of general rules of the four departments of the edition of Chinese pharmacopoeia 2015, and the results are shown in Table 1.

TABLE 1 detection results of ethanol extract from Lithospermum erythrorhizon Siebold et Zuccarini formula granule

As can be seen from the above table, the ethanol extract of the three batches of finished products is higher than 5.0%. Considering that the ethanol extract of the medicinal materials has certain fluctuation with the production place and the batch number, the ethanol extract of the lithospermum formula granules is temporarily specified to be not less than 5.0 percent.

Experimental example 1

A preparation method of radix Arnebiae granule comprises the following steps:

taking 10000g of lithospermum decoction pieces, adding water for decocting twice, filtering, concentrating the filtrate into clear paste, adding a proper amount of auxiliary materials, drying, adding the auxiliary materials, uniformly mixing, preparing 1000g of granules, and subpackaging to obtain the traditional Chinese medicine.

The quality standard of the lithospermum formula granules is as follows:

1. processing: removing impurities, and cutting into thick pieces or sections.

2. The preparation method comprises the following steps: taking 10000g of lithospermum decoction pieces, adding water for decocting twice, filtering, concentrating the filtrate into clear paste, adding a proper amount of auxiliary materials, drying, adding the auxiliary materials, uniformly mixing, preparing 1000g of granules, and subpackaging to obtain the traditional Chinese medicine.

3. The characteristics are as follows: the product is brown to black brown granules; special smell, slightly bitter taste.

4. And (3) identification:

grinding 2g of the product, adding 30ml of ethanol, heating and refluxing for 1 hour, filtering, evaporating the filtrate to dryness, and dissolving the residue in 2ml of methanol to obtain a sample solution. And adding water into 2.5g of radix Arnebiae control material, adding 30ml of water, filtering, evaporating the filtrate, and adding ethanol into the residue to 30ml to obtain control solution. Performing thin layer chromatography (0502 of the four ministry of the national pharmacopoeia 2015), collecting 10 μ l of each of the two solutions, developing with cyclohexane-toluene-ethyl acetate-formic acid (5: 0.5: 0.1) as developing agent, taking out, air drying, spraying 10% potassium hydroxide methanol solution, and displaying fluorescent spots of the same color in the chromatogram of the test solution at the position corresponding to the chromatogram of the control solution.

5. Examination of

Meets the regulations of granules (0104 in the four ministerial general rules of 2015, China pharmacopoeia).

6. Extract of plant

The product is ground into fine powder, about 2g of the powder is precisely weighed, 100ml of ethanol is precisely added, and the content is 11.45% by hot dipping method according to alcohol-soluble extract determination method (2201 in the four departments of the pharmacopoeia of China 2015).

7. Specification of

1g of the formula particle is equivalent to 10.0g of decoction pieces.