阅读说明：本技术 一种前胡超微粉体制备工艺及其质量控制方法 (Preparation process and quality control method of radix peucedani ultra-micro powder ) 是由 王斌 林钦贤 康志英 梁伟龙 全玉锦 张华勇 吴振斌 区秋华 于 2020-07-14 设计创作，主要内容包括：本发明公开了一种前胡超微粉体制备工艺及其质量控制方法,包括如下步骤：取前胡饮片,采用冷冻干燥干燥至水分≤7.0%；将干燥后的前胡饮片进行超微粉碎,得到粒径35～45μm的前胡超微粉体,包装,即得。本发明制备工艺采用了冷冻干燥和超微粉碎技术相结合,操作环境属于低温(-20～-30℃),冷冻干燥能瞬时干燥物料,且避免有效成分的破坏,超微粉碎技术能大大增加药物的比表面积,提高药物中有效成分的溶出速度和溶出率,使药物吸收更容易吸收。本发明采用高效液相色谱法对前胡超微粉体的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素等多成分进行定量测定,可以全面、客观、准确地控制前胡超微粉体的质量,确保工艺稳定,疗效确切。(The invention discloses a process for preparing peucedanum root ultra-micro powder and a quality control method thereof, comprising the following steps: taking radix Peucedani decoction pieces, and freeze-drying until the water content is less than or equal to 7.0%; and (3) carrying out superfine grinding on the dried radix peucedani decoction pieces to obtain radix peucedani superfine powder with the particle size of 35-45 mu m, and packaging to obtain the radix peucedani superfine powder. The preparation process of the invention adopts the combination of freeze drying and superfine grinding technology, the operation environment is at low temperature (-20-30 ℃), the freeze drying can instantly dry the materials and avoid the damage of the active ingredients, the superfine grinding technology can greatly increase the specific surface area of the medicine, improve the dissolution speed and dissolution rate of the active ingredients in the medicine and ensure that the medicine is easier to absorb. The invention adopts the high performance liquid chromatography to carry out quantitative determination on the multiple components of the peucedanum praeruptorum dunn A, the peucedanum praeruptorum dunn B, the peucedanum praeruptorum dunn C, the peucedanum praeruptorum dunn E and the like of the peucedanum praeruptorum dunn ultra-micro powder, can comprehensively, objectively and accurately control the quality of the peucedanum praeruptorum dunn ultra-micro powder, ensures the.)

1. A process for preparing radix peucedani ultra-micro powder is characterized by comprising the following steps:

(1) taking radix peucedani decoction pieces, and freeze-drying until the water content is less than or equal to 7.0% to obtain dried radix peucedani decoction pieces;

(2) and (3) carrying out superfine grinding on the dried radix peucedani decoction pieces to obtain radix peucedani superfine powder with the particle size of 35-45 mu m, and packaging to obtain the radix peucedani superfine powder.

2. The process for preparing superfine peucedanum root powder according to claim 1, wherein in step (1), the temperature of freeze-drying is-20 to-30 ℃, the freeze-drying time is 2 to 3 hours, and the freeze-drying pressure is 20 to 40 Pa.

3. The process for preparing superfine peucedanum root powder according to claim 1, wherein in the step (2), the superfine grinding equipment is a vibrating type drug superfine grinder, the superfine grinding temperature is-20 to-30 ℃, and the superfine grinding time is as follows: 20-25 min.

4. The process for preparing superfine radix Peucedani powder of claim 1, wherein in step (2), the packaging is made by vacuum-pumping/N-filling polyethylene plastic bag₂And (6) packaging.

5. The quality control method for preparing radix Peucedani superfine powder of any of claims 1-4, wherein four components of praeruptorin A, praeruptorin B, praeruptorin C and praeruptorin E are simultaneously measured by HPLC, specifically:

5.1 chromatographic conditions column: thermo acclaim TM120 (250 mm. times.4.6 mm, 5 μm); a detector: UV detector (321 nm); water is taken as a mobile phase A, acetonitrile is taken as a mobile phase B, and gradient elution is carried out according to the specification of the following table; column temperature: 30 ℃; flow rate: 1.0 ml/min;

time/min Mobile phase A/%) Mobile phase B/%) 0～10 70 30 15 40 60 16 35 65 20 25 75 28 25 75 40 15 85

5.2 preparation of reference solution A proper amount of praeruptorin A, praeruptorin B, praeruptorin C and praeruptorin E are precisely weighed, and methanol is added to prepare a mixed reference solution containing 50 mu g of praeruptorin A, 50 mu g of praeruptorin B, 80 mu g of praeruptorin C and 60 mu g of praeruptorin E in each 1 ml;

5.3 preparation of test solution 0.5g of sample powder is precisely weighed, placed in a conical flask with a plug, precisely added with 25ml of methanol, weighed, ultrasonically treated (power 250W, frequency 45 kHz) for 30min, cooled, weighed again, supplemented with methanol to reduce the weight loss, shaken up, filtered, and a subsequent filtrate is taken to obtain the test solution;

5.4 measuring the mixed reference solution by the measuring method, respectively absorbing different volumes according to the chromatographic conditions, and injecting the volumes into a high performance liquid chromatograph for measuring to obtain the product;

the superfine powder contains praeruptorin A (C) calculated on dry product₂₁H₂₂O₇) Not less than 1.50%, and contains praeruptorin B (C)₂₄H₂₆O₇) Not less than 0.45%, and contains praeruptorin C₂₂H₂₂O₈) Not less than 1.00%, and contains praeruptorin E (C)₂₄H₂₈O₇) Not less than 0.60%.

6. The method of claim 5, further comprising measuring seven performance indicators of angle of repose, bulk density, moisture, total ash, acid insoluble ash, extract yield.

Technical Field

The invention belongs to the technical field of processing of traditional Chinese medicine powder decoction pieces, and particularly relates to a preparation process of radix peucedani ultra-micro powder and a quality control method thereof.

Background

The peucedanum root has a long medicinal history in China, is a traditional Chinese medicine with a wide effect, and is used in a plurality of well-known Chinese patent medicines for reducing phlegm and relieving cough, such as jizhi syrup, perilla seed qi-lowering pills and the like. In recent years, the market has found that a few sources of goods meeting the requirements of pharmacopoeia are available, the quality of the spot check is unqualified frequently, and especially praeruptorin A and praeruptorin B in the content determination items, so that the national bureau also records the praeruptorin in the national evaluation variety of 2020, and clearly proposes that each traditional Chinese medicine decoction piece production enterprise strictly controls the product quality and avoids the unqualified phenomenon.

The reports of the traditional Chinese medicine superfine grinding technology begin after the middle of the 90 s, the traditional Chinese medicine superfine grinding technology is increased year by year, the traditional Chinese medicine superfine grinding technology is particularly rapidly increased in two years, and the traditional Chinese medicine superfine grinding powder is more and more emphasized. The technology can break the cell membrane or cell wall of the crude drug of plants and animals, so that the active ingredients of the drugs in the cells directly contact with the menstruum, thereby being beneficial to the maximum absorption and utilization. Therefore, in order to solve the problems of high unqualified content, large quality difference and uncertain drug effect of the current radix peucedani decoction pieces, and combined with the application of the current traditional Chinese medicine superfine grinding technology, the invention improves the dissolution speed and dissolution rate of active ingredients in the medicine by preparing the radix peucedani superfine powder decoction pieces, so that the medicine is more fully absorbed, thereby improving the bioavailability of the medicine and solving the problems.

Disclosure of Invention

In order to overcome the defects of the prior art, the invention mainly aims to provide a process for preparing the peucedanum ultra-micro powder, wherein the effective substances are maximally reserved, and the dissolution speed and the dissolution rate of the effective substances are obviously improved.

The invention also aims to provide a quality control method of the preparation process of the peucedanum root ultra-micro powder, which can comprehensively, objectively and accurately control the quality of the peucedanum root ultra-micro powder by establishing a multi-index evaluation method, thereby ensuring stable process and exact curative effect.

The invention is realized by the following technical scheme:

a process for preparing radix peucedani ultra-micro powder comprises the following steps:

(1) taking radix peucedani decoction pieces, and freeze-drying until the water content is less than or equal to 7.0% to obtain dried radix peucedani decoction pieces;

(2) and (3) carrying out superfine grinding on the dried radix peucedani decoction pieces to obtain radix peucedani superfine powder with the particle size of 35-45 mu m, and packaging to obtain the radix peucedani superfine powder.

Wherein in the step (1), the freeze-drying temperature is-20 to-30 ℃, the freeze-drying time is 2 to 3 hours, and the freeze-drying pressure is 20 to 40 Pa.

Wherein, in the step (2), the superfine grinding equipment is a vibrating type medicine superfine grinder, the superfine grinding temperature is-20 to-30 ℃, and the superfine grinding time is as follows: 20-25 min.

Wherein, in the step (2), the packaging is realized by adopting a polyethylene plastic bag for vacuumizing/filling N₂And (6) packaging.

In addition, the invention also discloses a quality control method of the preparation process of the peucedanum ultra-micro powder, which adopts an HPLC method to simultaneously determine four components of praeruptorin A, praeruptorin B, praeruptorin C and praeruptorin E, and specifically comprises the following steps:

5.1 chromatographic conditions column: thermo acclaim TM120 (250 mm. times.4.6 mm, 5 μm); a detector: UV detector (321 nm); water is taken as a mobile phase A, acetonitrile is taken as a mobile phase B, and gradient elution is carried out according to the specification of the following table; column temperature: 30 ℃; flow rate: 1.0 ml/min;

time/min	Mobile phase A/%)	Mobile phase B/%)
			0～10	70	30
15	40	60
			16	35	65
20	25	75
			28	25	75
40	15	85

5.2 preparation of reference solution A proper amount of praeruptorin A, praeruptorin B, praeruptorin C and praeruptorin E are precisely weighed, and methanol is added to prepare a mixed reference solution containing 50 mu g of praeruptorin A, 50 mu g of praeruptorin B, 80 mu g of praeruptorin C and 60 mu g of praeruptorin E in each 1 ml;

5.3 preparation of test solution 0.5g of sample powder is precisely weighed, placed in a conical flask with a plug, precisely added with 25ml of methanol, weighed, ultrasonically treated (power 250W, frequency 45 kHz) for 30min, cooled, weighed again, supplemented with methanol to reduce the weight loss, shaken up, filtered, and a subsequent filtrate is taken to obtain the test solution;

5.4 measuring the mixed reference solution by the measuring method, respectively absorbing different volumes according to the chromatographic conditions, and injecting the volumes into a high performance liquid chromatograph for measuring to obtain the product;

the superfine powder contains praeruptorin A (C) calculated on dry product₂₁H₂₂O₇) Not less than 1.50%, and contains praeruptorin B (C)₂₄H₂₆O₇) Not less than 0.45%, and contains praeruptorin C₂₂H₂₂O₈) Not less than 1.00%, and contains praeruptorin E (C)₂₄H₂₈O₇) Not less than 0.60%.

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

(1) the preparation process of the invention adopts the combination of freeze drying and superfine grinding technology, the operation environment is at low temperature (-20-30 ℃), the freeze drying can instantly dry the materials and avoid the damage of the active ingredients, the superfine grinding technology can greatly increase the specific surface area of the medicine, improve the dissolution speed and dissolution rate of the active ingredients in the medicine, make the medicine easier to absorb, and increase the curative effect.

(2) The invention adopts the high performance liquid chromatography to carry out quantitative determination on the multiple components of the peucedanum praeruptorum dunn A, the peucedanum praeruptorum dunn B, the peucedanum praeruptorum dunn C, the peucedanum praeruptorum dunn E and the like of the peucedanum praeruptorum dunn ultra-micro powder, can comprehensively, objectively and accurately control the quality of the peucedanum praeruptorum dunn ultra-micro powder, ensures the.

Drawings

FIG. 1 is an HPLC chromatogram of an ultrafine powder of Peucedanum praeruptorum obtained in example 1 of the present invention.

Detailed Description

The present invention is further illustrated by the following specific embodiments, which are not intended to limit the scope of the invention.

The raw materials used in the examples and comparative examples of the present invention were all commercially available.

Particle size: the particle size distribution is measured by BT-2001 laser particle size distribution instrument combined with microscopy, and D is used₉₀The value is used as an index for reflecting the uniformity of the particle size distribution and is applied to the powderThe situation is described.

Bulk density, angle of repose: and a BT-100 type powder comprehensive characteristic tester is adopted for measurement.

Moisture, total ash, acid insoluble ash, leachate: according to the regulation of 'Chinese pharmacopoeia' of 2015 edition, the content is detected and calculated according to the determination method of water, total ash, acid insoluble ash and extract under the item of peucedanum.

The extract yield is as follows: weighing 5.0g of radix peucedani ultra-micro powder decoction pieces, adding 18 times of boiling water for soaking for 30min at one time, filtering, and cooling to room temperature for later use. Precisely measuring 25ml, placing in an evaporation dish dried to constant weight, drying in a water bath, drying at 105 ℃ for 3h, cooling in a dryer for 30min, precisely weighing the mass, drying at 105 ℃ for 1h, cooling in the dryer for 30min, weighing the mass until the mass difference of 2 times is not more than 0.3mg, recording the mass of the extract of the sample, and calculating the yield of the extract.