阅读说明：本技术 一种快速评价中药配方颗粒内在成分和质量的方法 (Method for rapidly evaluating internal components and quality of traditional Chinese medicine formula granules ) 是由 宋细忠 李小丽 钱丽梅 陈述耀 郭磊夫 张景菊 于喆 尹炜 付农城 于 2020-09-01 设计创作，主要内容包括：本发明提供了一种快速评价中药配方颗粒内在成分和质量的方法,属于中药分析技术领域,包括以下步骤：1)采用紫外分光光度计法测定对照组样本内在成分的含量；2)对照组样本折光率的测定；3)待测样品质量判断：待测样品与对照组样本折光率比较；4)使用全波长紫外-可见吸收光谱仪,建立各成分含量与紫外-可见吸收光谱之间的关系曲线；5)配制与待测样品溶液,测定其紫外-可见吸收光谱,将得到的光谱信息输入步骤4)所得关系曲线中,计算待测样品中相应成分的含量。本发明可同时对多种成分进行定性和定量分析,与传统的分析方法相比,缩短测定时间80倍以上,操作简单、快速,可在中药配方颗粒制剂生产中推广应用。(The invention provides a method for rapidly evaluating the internal components and quality of traditional Chinese medicine formula granules, belonging to the technical field of traditional Chinese medicine analysis and comprising the following steps: 1) measuring the content of the internal components of the control group sample by adopting an ultraviolet spectrophotometer method; 2) measuring the refractive index of a control group sample; 3) and (3) judging the quality of the sample to be detected: comparing the refractive index of the sample to be detected with that of the reference group sample; 4) establishing a relation curve between the content of each component and the ultraviolet-visible absorption spectrum by using a full-wavelength ultraviolet-visible absorption spectrometer; 5) preparing a sample solution to be detected, measuring the ultraviolet-visible absorption spectrum of the sample solution, inputting the obtained spectrum information into the relation curve obtained in the step 4), and calculating the content of the corresponding component in the sample to be detected. The invention can carry out qualitative and quantitative analysis on a plurality of components simultaneously, shortens the determination time by more than 80 times compared with the traditional analysis method, has simple and quick operation, and can be popularized and applied in the production of the traditional Chinese medicine formula granular preparation.)

1. A method for rapidly evaluating the internal components and quality of traditional Chinese medicine formula granules is characterized by comprising the following steps:

1) and (3) determination of internal components and contents of the control group sample: taking the traditional Chinese medicine formula granules of the control group, and measuring the contents of the internal components by adopting an ultraviolet-visible spectrophotometer method;

2) measurement of refractive index of control sample: preparing a reference group sample into a solution with a certain mass concentration, and testing the refractive index of the solution to be A;

3) and (3) judging the quality of the sample to be detected: taking the traditional Chinese medicine formula particles to be tested, preparing a solution with the same mass concentration as that of a control group sample, and testing the refractive index of the solution to be tested to be B; if the A-B-A is less than or equal to 5 percent, preliminarily judging that the quality of the sample to be detected is qualified, and performing the operations of the steps 4) and 5); otherwise, the quality is unqualified;

4) establishing a relation curve of the content of each component and the ultraviolet absorption spectrum: acquiring ultraviolet-visible absorption spectrum data of a control group sample by using a full-wavelength ultraviolet-visible absorption spectrometer, and establishing a relation curve between the content of each component and the ultraviolet-visible absorption spectrum;

5) testing a sample to be tested: preparing a sample solution to be detected, measuring the ultraviolet-visible absorption spectrum of the sample solution, inputting the obtained spectrum information into the relation curve obtained in the step 4), and calculating the content of the corresponding component in the sample to be detected.

2. The method for rapidly evaluating the internal components and quality of the traditional Chinese medicine formula granules according to claim 1, wherein the quality judgment conditions in the step 3) are as follows: if the proportion of A-B-A is less than or equal to 3.5 percent, preliminarily judging that the quality of the sample to be detected is qualified, and carrying out the operations of the steps 4) and 5); otherwise, the quality is not qualified.

3. The method for rapidly evaluating the intrinsic components and quality of the Chinese medicinal granules according to claim 1, wherein the step 4) comprises placing a control sample diluent with a certain concentration in an ultraviolet-visible spectrometer for full-wavelength scanning, performing at least 3 parallel scans on each sample, and taking the average spectrum data as the control sample ultraviolet-visible absorption spectrum data.

4. The method for rapidly evaluating the internal components and quality of the traditional Chinese medicine formula granules according to claim 1, wherein the wavelength scanning range of the ultraviolet-visible absorption spectrum in the step 4) is 190-800 nm.

5. The method for rapidly evaluating the intrinsic ingredients and the quality of the TCM formula granules according to claim 1, wherein the quality index substances in the TCM formula granules in the step 4) are selected for establishing the relationship curve.

6. The method for rapidly evaluating the intrinsic components and quality of the traditional Chinese medicine formula granules according to claim 1, wherein the method for establishing the relationship curve in the step 4) comprises the following steps: and establishing a relation curve between the content of each component and the ultraviolet absorption spectrum by adopting a multivariate data analysis method.

7. The method for rapidly evaluating the intrinsic components and quality of Chinese medicinal granules according to claim 6, wherein the multivariate data analysis method is a principal component regression method or a partial least squares method.

8. The method for rapidly evaluating the intrinsic composition and quality of a Chinese medicinal granule according to claim 1, wherein the step 4) further comprises using leave-one-out cross-validation relationship curve.

9. The method for rapidly evaluating the intrinsic ingredients and the quality of the traditional Chinese medicine formula granules according to claim 1, wherein the correlation coefficient of the relation curve of the step 4) is not less than 0.95.

10. The method for rapidly evaluating the intrinsic ingredients and quality of the traditional Chinese medicine formula particle as claimed in claim 1, wherein the refractive index is measured by using a precision refractometer.

Technical Field

The invention relates to the technical field of traditional Chinese medicine analysis, in particular to a method for rapidly evaluating the internal components and quality of traditional Chinese medicine formula granules.

Background

In the production process of the traditional Chinese medicine formula granules, the quality control is a very critical step. In the prior art, methods for analyzing and detecting the quality of traditional Chinese medicines generally comprise a high performance liquid chromatography method, a mass spectrum fingerprint spectrum quality control method, a liquid chromatography-mass spectrum combined method, an ultraviolet spectrophotometry and the like. The method has high analysis precision, but needs a great deal of time for an analyst to analyze, has complex operation, long service time of the instrument, troublesome pretreatment and high requirements on the instrument and the analyst, and is not suitable for real-time analysis and monitoring in the production process.

Disclosure of Invention

The invention aims to solve the problems and provides a method for analyzing the quality of the traditional Chinese medicine formula granules, which is simple, quick and accurate to operate. The following technical scheme is adopted:

the invention provides a method for rapidly evaluating the internal components and quality of traditional Chinese medicine formula granules, which comprises the following steps:

1) and (3) determination of internal components and contents of the control group sample: taking the traditional Chinese medicine formula granules of the control group, and measuring the contents of the internal components by adopting an ultraviolet-visible spectrophotometer method;

2) measurement of refractive index of control sample: preparing a solution with a certain mass concentration from traditional Chinese medicine formula granules with known components and contents, and testing the refractive index of the solution to be A;

3) and (3) judging the quality of the sample to be detected: taking the traditional Chinese medicine formula particles to be tested, preparing a solution with the same mass concentration as that of a control group sample, and testing the refractive index of the solution to be tested to be B; if the A-B-A is less than or equal to 5 percent, preliminarily judging that the quality of the sample to be detected is qualified, and performing the operations of the steps 4) and 5); otherwise, the quality is unqualified;

4) establishing a relation curve of the content of each component and the ultraviolet absorption spectrum: acquiring ultraviolet-visible absorption spectrum data of a control group sample by using a full-wavelength ultraviolet-visible absorption spectrometer, and establishing a relation curve between the content of each component and the ultraviolet-visible absorption spectrum;

5) testing a sample to be tested: preparing a sample solution to be detected, measuring the ultraviolet-visible absorption spectrum of the sample solution, inputting the obtained spectrum information into the relation curve obtained in the step 4), and calculating the content of the corresponding component in the sample to be detected.

The method comprises the steps of firstly measuring the content of components in the traditional Chinese medicine formula particles by adopting an ultraviolet spectrophotometer method, then testing the refractive index of the traditional Chinese medicine formula particles, primarily judging the quality of the traditional Chinese medicine formula particles, then measuring the ultraviolet absorption spectrum data of the particles by adopting a full-wavelength ultraviolet absorption spectrometer, establishing a relation curve between the content of each component and an ultraviolet-visible absorption spectrum, and carrying out full-wavelength ultraviolet-visible spectrum analysis on the traditional Chinese medicine formula particles to be measured, wherein the internal components and the quality of the traditional Chinese medicine formula particles can be obtained from the relation curve. The invention can identify and analyze the quality of various particle components at one time, has simple operation and short instrument service time, can quickly obtain the components and quality results of the traditional Chinese medicine formula particles, and is convenient and quick.

Preferably, the quality judgment condition in step 3) is: if the proportion of A-B-A is less than or equal to 3.5 percent, preliminarily judging that the quality of the sample to be detected is qualified, and carrying out the operations of the steps 4) and 5); otherwise, the quality is not qualified.

Preferably, in the step 4), the control group sample diluent with a certain concentration is placed in an ultraviolet-visible spectrometer for full-wavelength scanning, a solvent for preparing the diluent is used as a blank reference solution, each sample is subjected to at least 3 times of parallel scanning, and average spectrum data is taken as control group sample ultraviolet-visible absorption spectrum data, so that the accuracy of a test result is ensured.

Preferably, the wavelength scanning range of the ultraviolet-visible absorption spectrum in the step 4) is 190-800 nm.

Preferably, the quality index substances in the traditional Chinese medicine formula granules are selected in the step 4) to establish a relation curve, so that the data analysis time is shortened, and the analysis efficiency is improved.

Preferably, the method for establishing the relationship curve in step 4) includes: and establishing a relation curve between the content of each component and the ultraviolet absorption spectrum by adopting a multivariate data analysis method.

Preferably, the multivariate data analysis method is a principal component regression method or a partial least squares method.

Preferably, the step 4) further comprises using leave-one-out cross-validation relationship curves.

Preferably, the correlation coefficient of the relation curve of the step 4) is more than or equal to 0.95.

Preferably, the refractive index is measured using a precision refractometer.

The invention can obtain at least one of the following beneficial effects:

1. the method provided by the invention can be used for qualitatively and quantitatively analyzing a plurality of components simultaneously, and solves the problem that the content of each component in the traditional Chinese medicine formula particles is difficult to be rapidly determined. Compared with the traditional analysis method, the method shortens the determination time by more than 80 times and has high efficiency.

2. The method provided by the invention has accurate analysis result, can effectively ensure the product quality of the traditional Chinese medicine formula granules, and can be used for the quality control of products.

3. The method provided by the invention does not need a large amount of organic solvent, and accords with the concept of green manufacturing.

4. The method provided by the invention is simple and rapid to operate, and can be popularized and applied in the production of the traditional Chinese medicine formula granular preparation.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The embodiment of the invention takes fried sophora japonica particles as experimental objects.

The information of the chemical reagents and experimental instruments used in the examples of the present invention is as follows:

reagent

Methanol (analytically pure, national group chemical reagent limited), ethanol (analytically pure, national group chemical reagent limited), distilled water (self-made), perchloric acid (analytically pure, national group chemical reagent limited), vanillin (analytically pure, shanghai alatin biochemical technology limited), glacial acetic acid (analytically pure, shanghai alatin biochemical technology limited), sodium nitrite (analytically pure, shanghai alatin biochemical technology limited), sodium hydroxide (analytically pure, tianjin Guangfu Jingfu Jing chemical institute), and aluminum nitrate (analytically pure, Tianjin Guangfu Jingfu Jing chemical institute).

Ginsenoside Re standard (China pharmaceutical and biological product institute), rutin control (batch number: 100080-one 201610, purity: for HPLC 91.9%, for UV 92.6%, China food and drug institute), 4.5% vanillin solution (weighing 5g vanillin, adding glacial acetic acid to dissolve and fixing volume to 100mL), and ginsenoside Re standard solution (accurately weighing 20.0mg ginsenoside Re standard, dissolving with methanol and fixing volume to 10 mL).

Second, experimental instrument

Ultraviolet-visible absorption spectrometer (BAGGI, Germany), precision refractometer (precision Abbe refractometer-NAR-3T), and ultraviolet-visible spectrophotometer (chromatography METASH, UV-5200 PC).