CN-122017164-A - Quality control method for processing process of nine-process rhizoma polygonati

CN122017164ACN 122017164 ACN122017164 ACN 122017164ACN-122017164-A

Abstract

The invention relates to the technical field of quality control of traditional Chinese medicine processing processes, in particular to a quality control method of a processing process of a nine-process rhizoma polygonati, which comprises a sample preparation step, a B element analysis step, a C electrochemical analysis step, a D thermogravimetric analysis step and an E data analysis step, wherein a quantitative association model between processing times and each parameter is established through cooperative application of three technologies of element analysis, electrochemical analysis and thermogravimetric analysis, so that scientific, objective and dynamic quality control and end point judgment of the processing process of the nine-process rhizoma polygonati are realized, the quality control efficiency is improved, and the cost is reduced.

Inventors

LING XU
HAO XINCAI
Xue Xuemei
LIU JINGJIAN

Assignees

湖北医药学院

Dates

Publication Date: 20260512
Application Date: 20260227

Claims (10)

1. A quality control method for a processing process of nine-process rhizoma polygonati is characterized by comprising the following steps: A. Sample preparation, namely taking rhizoma polygonati tubers of chicken heads, cleaning, steaming for nine times, and sun-drying for processing to respectively prepare 10 groups of samples of raw rhizoma polygonati and rhizoma polygonati from one time to nine time; B. The elemental analysis step comprises the steps of placing each group of sample powder into an elemental analyzer, taking helium as carrier gas and oxygen as combustion gas, and measuring the contents of five elements of carbon, hydrogen, nitrogen, sulfur and oxygen; C. Mixing each group of sample powder with an acidic cerium-malonic acid system, pre-reacting for 20-40 min in a constant-temperature water bath at 35-40 ℃, adding bromate solution to start reaction, and under the magnetic stirring condition, adopting differential pulse voltammetry scanning to record an electrochemical response curve and extracting oxidation peak potential and peak current value as characteristic parameters, wherein the acidic cerium-malonic acid system consists of sulfuric acid, ammonium cerium sulfate and malonic acid, and the mass-volume ratio of the sample powder to the system is 1:200-1:300 g/mL; D. Performing simultaneous thermogravimetric-differential scanning calorimetric analysis on each group of sample powder at room temperature to 800 ℃ with nitrogen as carrier gas and a heating rate of 10 ℃ per minute, and determining a total weight loss rate, a weight loss rate in a low-temperature area of 30 to 200 ℃, a weight loss rate in a medium-temperature area of 200 to 400 ℃, a residual rate above 400 ℃ and a decomposition peak temperature; E. And a data analysis step of carrying out correlation analysis on the processing times, the element content, the electrochemical oxidation peak current value and the thermogravimetric parameter by utilizing a multivariate statistical method, establishing a quantitative correlation model between the processing times, the element content, the electrochemical oxidation peak current value and the thermogravimetric parameter, and carrying out dynamic evaluation and end point judgment on the processing progress based on the model.
2. The quality control method of a processing process of nine-process rhizoma Polygonati of claim 1, wherein the processing process of nine-process rhizoma Polygonati specifically comprises the following steps: s1, cleaning, namely taking rhizoma polygonati tubers with chicken heads, removing impurities and fibrous roots, putting the rhizoma polygonati tubers into a roller medicine washing machine, repeatedly washing the rhizoma polygonati tubers, spreading and airing the rhizoma polygonati tubers until the quality becomes soft, and washing surface floating dust with clear water again; s2, steaming the washed raw rhizoma polygonati with the surface dried in the shade in a water-proof manner, covering the raw rhizoma polygonati during steaming, heating the raw rhizoma polygonati to the internal steam of a pot by strong fire at 150-220 ℃, and continuously steaming the rhizoma polygonati for 8 hours by slow fire at 80-120 ℃ so as to ensure that bottom water is not dried in time during steaming; S3, stewing and drying, namely stopping heating after steaming, stewing for 10 hours by using waste heat in a pot until the color of the rhizoma polygonati turns into yellow brown, taking out, placing in a clean baking tray, drying for 6 hours in a 60 ℃ hot air circulation drying oven, cooling overnight, and finishing the first steaming to obtain the rhizoma polygonati; S4, circularly processing, namely spraying clear water to moisten the surface of the rhizoma polygonati before steaming for the second time to the ninth time, repeating the steaming, stewing and drying processes of the step S2 and the step S3 for 8 times, directly cooling after steaming for the ninth time, cutting into slices, and drying in a 60 ℃ hot air circulation drying box to constant weight to obtain a finished product of the rhizoma polygonati for nine times.
3. The quality control method of a processing process of nine-process rhizoma Polygonati of claim 1, wherein the specific conditions of the elemental analysis are: sample pretreatment, namely drying a sample at 40 ℃ for 8 hours, drying the sample at 50 ℃ for 8 hours and drying the sample at 60 ℃ to constant weight, crushing the sample, and sieving the crushed sample with a 60-100-mesh sieve; The instrument conditions are that helium is taken as carrier gas and oxygen is taken as combustion gas, the contents of five elements of carbon, hydrogen, nitrogen, sulfur and oxygen are measured, and the results are expressed in weight percent.
4. The quality control method of a processing process of nine-process rhizoma Polygonati of claim 1, wherein the specific conditions of the electrochemical analysis are: sample pretreatment, namely screening the rhizoma polygonati powder by a 60-100-mesh sieve, and drying the rhizoma polygonati powder to constant weight at 40-60 ℃; The detection condition is that the constant temperature is 35-39 ℃, the magnetic stirring rotating speed is 400-600 r/min, the pre-reaction time is 25-35 min, a three-electrode system is adopted, wherein the working electrode is a glassy carbon electrode, the counter electrode is a platinum wire electrode, and the reference electrode is a saturated calomel electrode; The reagent mixture ratio is that rhizoma polygonati powder 0.08-0.12 g, 2.5-3.5 mol/L sulfuric acid solution 12mL, 0.004-0.006mol/L ceric ammonium sulfate solution 3.0mL, 0.35-0.45 mol/L malonic acid solution 6.0mL, 0.15-0.25 mol/L sodium bromate solution 3.0mL; The measuring method comprises the steps of adopting a differential pulse voltammetry, scanning the potential range to be 0.5-1.5V, the pulse amplitude to be 0.05V, the pulse width to be 0.05s, the sampling interval to be 0.02s, the sensitivity to be 0.001A/V, and recording the oxidation peak potential and the peak current value.
5. The quality control method of a processing process of nine-process rhizoma Polygonati of claim 1, wherein the specific conditions of the thermogravimetric analysis are as follows: the temperature range is room temperature to 800 ℃; The temperature rising rate is 10 ℃ per minute; Carrier gas, nitrogen; measuring parameters including a TG curve, a DTG curve and a DSC curve; The key indexes are total weightlessness, weightlessness in a low-temperature region of 30-200 ℃, weightlessness in a medium-temperature region of 200-400 ℃, residual rate above 400 ℃ and main decomposition peak temperature.
6. The quality control method of a processing process of nine-process rhizoma Polygonati according to claim 1, wherein the element index judgment criteria of the processing end point of nine-process rhizoma Polygonati are: the carbon content is more than or equal to 42 percent, the nitrogen content is more than or equal to 2.0 percent the sulfur content is less than or equal to 0.15 percent.
7. The quality control method of a processing process of nine-process rhizoma Polygonati according to claim 1, wherein the electrochemical index determination criteria of the processing end point are: the first oxidation peak current value is less than or equal to 1.8X10- 4 A, and the first oxidation peak potential value is within the range of 0.10-0.13V.
8. The quality control method of a processing process of nine-process rhizoma Polygonati according to claim 1, wherein the thermal weight index judgment criteria of the processing end point are: The residual mass at 200 ℃ is more than or equal to 60%, the total weight loss rate is less than or equal to 72%, and the residual rate above 400 ℃ is more than or equal to 34%.
9. The method for quality control of a processing process of nine-process rhizoma Polygonati according to claim 1, wherein the correlation index judgment criteria of the processing end point is: The correlation coefficient r of the processed times and the Szellman grade of the current value of the first oxidation peak and the total weight loss rate is less than or equal to-0.85.
10. The method for quality control of a processing process of nine-process rhizoma Polygonati of claim 1, wherein the multivariate statistical method comprises a Pearson correlation analysis, a Szelman scale correlation analysis, and a linear regression analysis.

Description

Quality control method for processing process of nine-process rhizoma polygonati Technical Field The invention belongs to the technical field of traditional Chinese medicine quality control, and particularly relates to a method for dynamically monitoring and judging an endpoint of a processing process of nine-process rhizoma polygonati based on a multidimensional analysis technology. Background In the 2020 edition of Chinese pharmacopoeia, the traditional Chinese medicine rhizoma Polygonati is dried rhizome of Polygonatum kingianum Polygonatum kingianum Coll. Et Hemsl. Of Liliaceae, polygonatum sibiricum Polygonatum sibiricum Red or Polygonatum cyrtonema Polygonatum cyrtonema Hua, which is known as Polygonatum sibiricum, and Polygonatum sibiricum in different shapes, is picked and excavated in spring and autumn to remove fibrous roots, cleaned, placed in boiling water and slightly scalded or steamed until the heart is penetrated, and then dried; Rhizoma Polygonati has effects of invigorating qi, nourishing yin, invigorating spleen, moistening lung, and invigorating kidney. In 3 months 2002, the ministry of original health issues a list of articles, which are both foods and medicines, and rhizoma Polygonati is listed therein. However, the rhizoma polygonati contains more calcium oxalate crystals, and people feel numbness of the mouth and tongue and irritation to the throat when taking the rhizoma polygonati directly, so the rhizoma polygonati is not suitable for direct use, and the rhizoma polygonati used in production and life is a processed product; According to ancient books, the processing of rhizoma polygonati starts in Liu Song th south China (420-479 years), and the Tang dynasty 'diet therapy herbal medicine' firstly proposes a rhizoma polygonati nine-steaming and nine-sun-drying method, so that the nine-steaming and nine-sun-drying processing technology of rhizoma polygonati is primarily formed and is used up to now. However, the process control of the existing nine-steaming and nine-sun drying process depends on experience and sensory judgment of a processor, lacks scientificity and rationality, and makes the quality of the final finished product of the nine-processed rhizoma polygonati very different among batches; The quality control method of the nine-process rhizoma polygonati mainly comprises the following steps: (1) The analysis methods based on chemical components such as Zhang Xiaoyan and the like (CN 116370572A), li Mengen and the like (Shizhen national medicine, 2021, volume 32, 8 th phase 1897-1900 pages), hu Changjiang and the like (CN 201810690896.9) are disclosed, and high performance liquid chromatography is adopted to measure the content of 5-hydroxymethylfurfural (5-HMF), polysaccharide and monosaccharide, and an image analysis technology is combined to measure the total color value, wherein the methods can reflect part of the chemical component changes, but the sample pretreatment is complex, the detection time is long (usually several hours), and the requirements of quick and continuous monitoring on a processing site cannot be met. Meanwhile, the single component index cannot comprehensively reflect the complex material conversion and structural change in the processing process; (2) An experience judging method based on sensory characteristics, such as DB 4203/T239-2024, rhizoma Polygonati nine-steaming and nine-sun processing technical procedure, mainly relies on experience and sensory of a processor to judge, lacks scientificity and objectivity, and has large quality difference between batches; (3) Polysaccharide component based analysis methods such as bear sail (modern food technology, volume 38, pages 9, 171-180 of 2022) analyze polysaccharide molecular weight distribution and monosaccharide composition by size exclusion gel chromatography and ion chromatography, and focus on polysaccharide structural analysis, and fail to fully reflect element composition and thermodynamic property changes in the processing process; In summary, the prior art has the following defects of (1) lack of systematic research on element composition change in a processing process, (2) lack of a quick and simple electrochemical detection method, (3) lack of a processing process dynamic monitoring method based on a thermal analysis technology, (4) lack of a correlation analysis method of multidimensional analysis parameters, and (5) limitations of the prior electrochemical detection technology, wherein the prior art mainly comprises two types of ① polysaccharide quantitative detection (such as CN 202510970576.9) based on a molecularly imprinted sensor, an AC-COOH-PANI composite material modified electrode is required to be prepared, a high-selectivity identification interface is designed only for a single known target (such as polysaccharide), the electrode is subjected to endpoint quantitative detection, the electrode modification process is complex, the cost is high, the universality is low, ② elect