阅读说明：本技术 一种红景天配方颗粒的质量标准检测方法 (Quality standard detection method for rhodiola rosea formula granules ) 是由 李刚 周云雷 孟瑞 王新灵 刘远 李冬梅 于 2020-05-11 设计创作，主要内容包括：本发明公开了一种红景天配方颗粒的质量标准检测方法,包括红景天配方颗粒的鉴别、红景天配方颗粒的检查、红景天配方颗粒相关物质的含量测定。本发明针对红景天配方颗粒提供了系统化,科学化的质量标准检测方法,包括其鉴别、各项理化指标的检查以及相关成分含量的测定,测定方法使用参数精准控制,能完全反应出红景天配方颗粒的质量,更有效地控制产品质量,并可作为大规模生产的红景天配方颗粒疗效一致性的评价依据,具有较高的科学指导和产业调控价值。(The invention discloses a quality standard detection method of rhodiola rosea formula granules, which comprises the steps of identifying the rhodiola rosea formula granules, checking the rhodiola rosea formula granules and measuring the content of related substances of the rhodiola rosea formula granules. The invention provides a systematic and scientific quality standard detection method aiming at rhodiola rosea formula granules, which comprises the steps of identification, check of various physical and chemical indexes and determination of related component content, and the determination method adopts accurate control of parameters, can completely reflect the quality of the rhodiola rosea formula granules, more effectively controls the product quality, can be used as an evaluation basis for the consistency of the curative effect of the rhodiola rosea formula granules produced in large scale, and has higher scientific guidance and industrial regulation and control values.)

1. A quality standard detection method of rhodiola rosea formula granules is characterized by comprising the following steps:

(1) identifying the rhodiola rosea formula particles;

(2) checking the rhodiola rosea formula particles;

(3) and (4) measuring the content of related substances of the rhodiola rosea formula granules.

2. The quality standard testing method of rhodiola rosea formula granules according to claim 1, wherein the identification method comprises the following steps:

(1) the characteristics are as follows: the granules are reddish brown to brown, fragrant, slightly bitter and astringent in taste and sweet after taste;

(2) taking a proper amount of salidroside reference substance, precisely weighing, and adding methanol to obtain a solution containing 0.5mg per 1ml to obtain reference substance solution;

(3) taking a proper amount of rhodiola rosea formula particles, grinding, taking 0.2g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of methanol, sealing the plug, weighing, carrying out ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, taking a subsequent filtrate, and obtaining a test solution for later use;

(4) absorbing 10 μ 1 of each of the reference solution and the sample solution by thin layer chromatography, respectively dropping on the same silica gel G thin layer plate, developing with developing agent, taking out, air drying, fumigating in iodine vapor, and displaying spots of the same color in the sample chromatogram at the position corresponding to the reference chromatogram.

3. The quality standard detection method for rhodiola rosea formula particles according to claim 2, wherein the developing solvent in the step 4 is chloroform, methanol, acetone and water according to a volume ratio of 6: 3: 1: 1, the lower layer solution of the mixture.

4. The method for testing the quality standard of rhodiola rosea formula granules according to claim 1, wherein the inspection method comprises the following steps:

(1) and (3) checking the granularity: according to the particle size and particle size distribution determination method, the sum of the first sieve and the fifth sieve which can not pass through the sieve can not exceed 15 percent;

(2) and (3) moisture inspection: the content of the Chinese medicinal granule is not more than 8.0% by water content determination method;

(3) and (3) testing the dissolubility: taking 10g of a test sample, adding 200ml of hot water, stirring for 5 minutes, immediately observing, and completely dissolving or slightly turbidity without foreign matters such as coke breeze and the like;

(4) and (3) microbial limit inspection: according to the microbial limit test method, the number of aerobic bacteria is regulated to be less than 10³cfu/g, the number of mould and yeast is not more than 10²cfu/g, Escherichia coli could not be detected;

(5) heavy metal and harmful element inspection: according to the determination of the method for measuring lead, cadmium, arsenic, mercury and copper, lead can not exceed 5mg/kg, cadmium can not exceed 0.3mg/kg, arsenic can not exceed 2mg/kg, mercury can not exceed 0.2mg/kg and copper can not exceed 20 mg/kg;

(6) checking extract: it is measured by hot dipping method of alcohol-soluble extract measurement method, using ethanol as solvent, and should not be less than 18.0%.

5. The method for detecting the quality standard of rhodiola rosea formula granules according to claim 1, wherein the content measurement comprises the following steps:

(1) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as filler, methanol-water (15: 85) is used as mobile phase, the detection wavelength is 275nm, the column temperature is 30 ℃, the flow rate is 1.0ml/min, and the number of theoretical plates is not less than 2000 calculated according to the salidroside peak;

(2) preparation of control solutions: taking a proper amount of salidroside reference substance, precisely weighing, and adding methanol to obtain solution containing 0.5mg per 1 ml;

(3) preparation of a test solution: taking a proper amount of rhodiola rosea formula particles, grinding, taking 0.2g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of methanol, sealing the plug, weighing, carrying out ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the rhodiola rosea formula particle;

(4) the determination method comprises the following steps: precisely sucking 5 μ l of each of the control solution and the sample solution, respectively, injecting into a liquid chromatograph, and measuring, wherein the content of salidroside in each 1g is not less than 10.8mg, calculated according to the dry product.

Technical Field

The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to a quality standard detection method of rhodiola rosea formula granules.

Background

The radix Rhodiolae granule is prepared from dried root and rhizome of Rhodiola crenulata Rhodiola crenulata (hook.f. ETThoms.) H.Ohba of Crassulaceae, has sweet, bitter and flat taste, and has effects of invigorating qi, promoting blood circulation, dredging collaterals and relieving asthma, and can be used for treating qi deficiency, blood stasis, thoracic obstruction, cardiodynia, apoplexy, hemiplegia, listlessness and asthma.

In recent years, continuous development and research are carried out at home and abroad aiming at the efficacy and the effect of the rhodiola rosea serving as a medicinal material respectively, and a scheme of more cooperative treatment is expected to be found, so that the rhodiola rosea serving as a medicinal material can fully help patients in need to solve the problems on health. However, researches show that the properties of the main active ingredient salidroside of rhodiola are unstable, so that the traditional rhodiola formula granules not only have high impurity content and are inconvenient to carry and take, but also have low stability and are difficult to store. Meanwhile, no related quality standard detection method exists, the effective components of the method cannot be correspondingly guaranteed, and the safety and effectiveness of the medicine for patients are difficult to guarantee.

Disclosure of Invention

The invention aims to make up for the defects of the prior art and provides a quality standard detection method of rhodiola rosea formula granules.

In order to achieve the above object, the present invention provides the following technical solutions:

a quality standard detection method of rhodiola rosea formula granules comprises the following steps:

(1) identifying the rhodiola rosea formula particles;

(2) checking the rhodiola rosea formula particles;

(3) and (4) measuring the content of related substances of the rhodiola rosea formula granules.

Further, the authentication method comprises the following steps:

(1) the characteristics are as follows: the granules are reddish brown to brown, fragrant, slightly bitter and astringent in taste and sweet after taste;

(2) taking a proper amount of salidroside reference substance, precisely weighing, and adding methanol to obtain a solution containing 0.5mg per 1ml to obtain reference substance solution;

(3) taking a proper amount of rhodiola rosea formula particles, grinding, taking 0.2g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of methanol, sealing the plug, weighing, carrying out ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, taking a subsequent filtrate, and obtaining a test solution for later use;

(4) absorbing 10 μ 1 of each of the reference solution and the sample solution by thin layer chromatography, respectively dropping on the same silica gel G thin layer plate, developing with developing agent, taking out, air drying, fumigating in iodine vapor, and displaying spots of the same color in the sample chromatogram at the position corresponding to the reference chromatogram.

Preferably, the developing solvent in the step 4 is chloroform, methanol, acetone and water in a volume ratio of 6: 3: 1: 1, the lower layer solution of the mixture.

Further, the inspection method includes the steps of:

(1) and (3) checking the granularity: according to the particle size and particle size distribution determination method, the sum of the first sieve and the fifth sieve which can not pass through the sieve can not exceed 15 percent;

(2) and (3) moisture inspection: the content of the Chinese medicinal granule is not more than 8.0% by water content determination method;

(3) and (3) testing the dissolubility: taking 10g of a test sample, adding 200ml of hot water, stirring for 5 minutes, immediately observing, and completely dissolving or slightly turbidity without foreign matters such as coke breeze and the like;

(4) and (3) microbial limit inspection: according to the microbial limit test method, the number of aerobic bacteria is regulated to be less than 10³cfu/g, the number of mould and yeast is not more than 10²cfu/g, Escherichia coli could not be detected;

(5) heavy metal and harmful element inspection: according to the determination of the method for measuring lead, cadmium, arsenic, mercury and copper, lead can not exceed 5mg/kg, cadmium can not exceed 0.3mg/kg, arsenic can not exceed 2mg/kg, mercury can not exceed 0.2mg/kg and copper can not exceed 20 mg/kg;

(6) checking extract: it is measured by hot dipping method of alcohol-soluble extract measurement method, using ethanol as solvent, and should not be less than 18.0%.

Further, the content determination comprises the following steps:

(1) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as filler, methanol-water (15: 85) is used as mobile phase, the detection wavelength is 275nm, the column temperature is 30 ℃, the flow rate is 1.0ml/min, and the number of theoretical plates is not less than 2000 calculated according to the salidroside peak;

(2) preparation of control solutions: taking a proper amount of salidroside reference substance, precisely weighing, and adding methanol to obtain solution containing 0.5mg per 1 ml;

(3) preparation of a test solution: taking a proper amount of rhodiola rosea formula particles, grinding, taking 0.2g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of methanol, sealing the plug, weighing, carrying out ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the rhodiola rosea formula particle;

(4) the determination method comprises the following steps: precisely sucking control solution and sample solution respectively by 5 μ l, injecting into liquid chromatograph, and measuring to obtain dry extract containing salidroside (C) per 1g₁₄H₂₀O₇) Not less than 10.8 mg.

The invention has the advantages that:

the invention provides a systematic and scientific quality standard detection method aiming at rhodiola rosea formula granules, which comprises the steps of identification, check of various physical and chemical indexes and determination of related component content, and the determination method adopts accurate control of parameters, can completely reflect the quality of the rhodiola rosea formula granules, more effectively controls the product quality, can be used as an evaluation basis for the consistency of the curative effect of the rhodiola rosea formula granules produced in large scale, and has higher scientific guidance and industrial regulation and control values.

Drawings

FIG. 1 shows the results of the durability test in which the thin-layer plate 1 is a silicone G plate.

FIG. 2 shows the results of the durability test in which the thin-layer plate 2 is a silicone G plate.

FIG. 3 shows the results of durability tests of the thin-layer plates at 16.5 ℃ and 46% humidity.

FIG. 4 shows the results of durability tests of the thin-layer plates at a temperature of 40.0 ℃ and a humidity of 75%.

Fig. 5 is a graph showing the absorbance standard curve of lead standards at different concentrations.

FIG. 6 is a graph showing the absorbance standard curve of cadmium standards at different concentrations.

FIG. 7 is a graph showing the absorbance standard of arsenic standards at different concentrations.

FIG. 8 is a graph showing absorbance standards for various concentrations of mercury standards.

FIG. 9 is a graph showing absorbance standards for various concentrations of copper standards.

FIG. 10 shows the comparison of control, sample, adjuvant, and blank HP L C in the determination of salidroside content.

FIG. 11 is a graph showing the standard curve of salidroside.

FIG. 12 shows a durability test of L oT15497 chromatography column.

FIG. 13 shows a durability test of an S/N4 DG70770 column.

FIG. 14 shows L N B18123 column durability test.

Detailed Description

The technical scheme of the invention is further explained by combining the specific examples as follows: