CN111795877A - Digital quality control method for chromaticity of fructus psoraleae - Google Patents

Abstract

A chromaticity digital quality control method of Psoraleae, which is used to identify the processing quality of Psoraleae through a chromaticity digital method, mainly comprising: using a stimulus value direct reading method or a spectrophotometric method to measure tristimulus values X, Y, Z; 3) Calculate the tristimulus values X, Y, Z to give L ^* , a ^* , b ^* ; 4) Judge the psoralen medicinal material or the decoction piece by the position of L ^* , a ^* , b ^* in the coordinate system quality. The chromaticity of Psoraleae can easily distinguish Psoralea varieties and different processing methods, and is especially effective for identifying Psoralea decoction pieces and processed products. The method has the advantages of simple operation, shortened time, low cost, feasibility and widespread popularization, and can be used as a basis for quality evaluation of the processing of Psoraleae medicinal materials.

Description

A kind of psoralen chromaticity digital quality control method

technical field

The invention relates to a method for identifying traditional Chinese medicinal materials, and more particularly to a method for digital quality control of psoralen chroma.

Background technique

Chinese medicinal materials are fresh products or simply processed medicinal parts derived from plants, animals and minerals, and are directly used in medical care or as natural medicines as raw materials for medicine. There are many foreign medicines with the same name in Western medicine; similar products and counterfeit products are prone to appear in the market; in the same variety of Chinese medicinal materials, the quality of each individual is different; The "yield" of Chinese medicinal materials is uncontrollable; it is difficult to maintain the stability of the price. The quality is unstable, and the output and price are also unstable; but on the other hand, the slow, continuous, alleviating effect and effect; corresponding to the disease and constitution, with few side effects, stop the drug Post-symptoms were stable. In particular, the effect is guaranteed based on the long-standing clinical experience of traditional Chinese medicine theory.

Problems existing in Chinese herbal medicines as medicines: Chinese herbal medicines with the same origin as medicine and food should be selected from the origin and quality guaranteed. Chinese herbal medicines are multi-component complexes, which show their efficacy through the interaction between the components. It is not easy to accurately identify and evaluate a Chinese herbal medicine.

Identification and evaluation methods of Chinese herbal medicines: Chinese herbal medicines have a long history. The identification and evaluation of Chinese herbal medicines are mainly based on observation, and then analyzed by chemical reactions, pathological modeling reactions, chemical components and genes. (Table 1)

Table 1. Characteristics of various identification and quality assessment methods

The evaluation methods currently under study involve many aspects, but it can be said that a decisive and effective evaluation method is still being explored. At this time, it makes sense to use the evaluation method since ancient times. In the past, the identification and quality evaluation of Chinese herbal medicines were based on the color, smell, taste, touch, shape, size and severity of Chinese herbal medicines by experienced and skilled people. Plants are different in color, smell, taste, touch and so on. The ancients learned from the accumulated experience and were able to identify the differences in the characteristics of the varieties, and then based on the rich experience in practicing medicine, the subtle differences of the same medicinal materials were used as clues to select Chinese medicinal materials with curative effects.

However, people's sense organs and perception abilities are different, and different people's states will also affect the judgment results. Relying on the senses of color, smell, taste, touch, etc. to judge the same object, the person who makes the judgment and his own state and the environment at that time have different perceptions of aroma and taste. In addition, the current pharmacopoeia of each country also publishes color, odor, and taste as information that can be used for identification. However, almost all the color expressions in the pharmacopoeia are idioms, and the expressions are inconsistent. And the interpretation of color expression in customary sentences varies from person to person.

In order to make use of the ancient identification methods, it is necessary to objectively recognize the color and lustre, and objectively express a unified representation. And crude drug resources are not only considered domestic problems in China, but should be considered as medicinal resources circulating in the world. Therefore, it is expected that there will be a unified world standard for the expression of the color of Chinese medicinal materials.

To display the color of Chinese herbal medicines, "Chinese herbal medicines", "Light source", and "Sightseeing" are required. Chinese herbal medicines absorb part of the light from the irradiated light source and reflect the excess light. When reflected light enters the line of sight, people perceive light of a specific wavelength as a color. Due to the reflection of objects, vision can distinguish colored light, which intersects with various wavelength components. What we can see is light with wavelengths in the visible light range (380nm to 780nm). However, light is not a color. Light is defined as "stimulating the retina of the eye to cause visual radiation." Light entering the eye causes the retina to be stimulated, and the brain responds to it. The perception of "red", "cyan" and "green" (the three primary colors) in the spectrum is all on our retina, so the concept of color is born.

Observation of Chinese herbal medicines under different light sources, Chinese herbal medicines with different surface shapes, different observation directions, different lighting positions, the size of Chinese herbal medicines, indoor light and shade and temperature, etc. Regular reflection and absorption cause visual difference, etc., and the same color looks different.

For example, the area of the Chinese herbal medicine is larger than the smaller, and it feels bright (the area effect of the color), and the Chinese herbal medicine on a bright background is different in color than the dark background (contrast effect).

The terminology for color changes over time. The customary color names such as coral and pink can be used. System color names such as dark red and bright red are prefixed with adjectives before the system color name, and all colors can be classified and represented systematically. In short, accurate representation of colors is difficult to achieve. Therefore, it is expected to formulate their own unique standards for hue, lightness, and chroma to digitize colors to avoid misunderstandings in understanding.

The study of using color as a system to establish a numerical representation, that is, the study of formulating color standards was first proposed by the American painter Albert H. Mansell in 1905, and then he created different [hue] [lightness] [chroma]. The "Mansell Color System" that is used to classify and express colors using color paper, uses hue (H), lightness (V), and chroma (C) classification chips to interpret colors by code.

In modern times, an international consultative body related to color and light, the International Organization for Standardization, established the International Commission on Illumination (CIE: Commission International de I'Eclairege). CIE formulated the "XYZ (Yxy) color system" in 1931, and the "L*a*b* color system (CIE1976Lab color system)" in 1976. The adoption of these colorimetric systems makes it possible to express uniform chromaticity worldwide.

In addition to the above, the current types of color systems include RGB color system, xyY color system, Ostwald color system, NCS (Natural Color System) color system, DIN color system, RGBA color system. Color system, CMY color system, CMYK color system, CMK color system, HSV color system, HLS color system, etc. Among them, the most widely used is the "L*a*b* color system (CIE1976Lab color system). system)". At present, the visual inspection method is the most commonly used, with low cost and simple operation. However, this method only relies on the experimenter's senses to judge the quality of the drug, and is easily affected by the experimenter's subjective influence, so it is not scientific and rigorous; UV-Vis spectrophotometry is usually selected in a certain The color of the drug solution is measured at a specific wavelength. In fact, the composition of traditional Chinese medicine preparations is complex, and the color of the drug solution is the result of the interaction of different wavelengths. Therefore, the color of the drug solution cannot be accurately reflected by the absorbance value of a specific wavelength.

The processing of traditional Chinese medicine is guided by the theory of syndrome differentiation and treatment of traditional Chinese medicine, and the pharmaceutical technology is adopted according to the needs of drug use or the nature and flavor of the drug itself, as well as the different needs of preparations; it is a scientific system formed by traditional Chinese medicine through thousands of years of practical demonstrations; it is traditional Chinese medicine. The embodiment of continuous inheritance and innovation. Psoralea is a traditional bulk medicinal material in my country. It has the effects of invigorating Qi and relieving asthma, warming kidney and helping yang, warming spleen and stopping diarrhea. As early as "Kaibao Materia Medica" has medicinal records, it has a history of more than one thousand years of medicinal use. Modern research shows that its main index components (coumarins, flavonoids, terpene phenols, etc.) have estrogen-like, antibacterial, antitumor, antidepressant, antioxidant and other biological activities. But psoralen is dry and poisonous, and it is easy to hurt the yin and help the fire. Modern research has shown that the toxic components in Psoraleae can cause pathological changes in the kidneys, and progressive kidney damage can be seen in large doses. Therefore, many clinical drugs need to be concocted to achieve the purpose of increasing efficacy and reducing toxicity.

The processing method of psoraleae was first recorded in the Southern and Northern Dynasties "Leigong Processing Theory". The salt-burning method was first seen in the "Jufang" of the Song Dynasty, which was proposed to improve the Leigong processing method with complex processing technology. Later, in the Yuan Dynasty "Confucianism", there was also a record of the processing method of adding salt, frying, and reducing poison. In the Ming Dynasty, the method of salt-roasting has been greatly developed. In the "Forbidden Prescription", it is immersed in salt water for baking, and in "Shou Shi Bao Yuan", it is fried in salt water. In the Qing Dynasty, there were records of "soaking for one night", "soaking for one day" and "soaking for three days", and records of hot soaking in salt soup. The step-by-step improvements made by later generations of physicians in salt roasting, such as "micro-fried", "salted stir-fry", "salt-soaked stir-fry", and "combined with other medicines" are all aimed at removing dryness and toxins.

Since the 1963 edition of the "Chinese Pharmacopoeia", there has been a collection of the processing items of Psoraleae. Let cool, let dry, and serve. The following three editions of the Pharmacopoeia added the method of "spraying salt water evenly" in the processing. By the 1990 edition of the Pharmacopoeia, the content of the salt-burning method was slightly changed and gradually refined. Since the 1990 edition, the processing method of Psoraleae has been implemented under the salt-burning method in the General Principles of Processing in the appendix of the Chinese Pharmacopoeia.

SUMMARY OF THE INVENTION

Bakuchiol is the toxic component of Bakuchiol, which accounts for more than 50% in the Bakuchiol ether extract, and is the main substance in the adverse reaction of Bakuchiol; the above-mentioned Bakuchiol commercially available decoction pieces and raw medicinal materials and salts It is difficult to distinguish the sunburned products. In the present invention, the color of the original Psoraleae medicinal material and the extract is measured by a colorimeter, and the toxicity of the decoction pieces of Psoralea japonicus is judged. The provided digital quality control method for psoralen chroma uses a specific point in the CIE Lab three-dimensional coordinates to represent a specific color by relying on the CIELab color space. Include the following steps:

1) pulverize the Psoraleae medicinal material or decoction pieces to obtain the material to be inspected;

2) The material to be tested is placed in a cuvette, and the tristimulus values X, Y, and Z are measured by the direct reading method of the stimulus value or the spectrophotometric method;

3) Calculate the tristimulus values X, Y, and Z to give L ^* , a ^* , b ^* ;

4) Judging the quality of Psoraleae medicinal materials or decoction pieces by the positions of L ^* , a ^* , b ^* in the coordinate system.

Measurement conditions are: diffuse illumination; reflected light; light source: ID65 light; observation field: 10°; color system: CIE L*a*b* color system; start and end wavelength: 780～360nm; ; Slit width: 1nm; Special cuvette 12mm*10mm; Measurement value: the average value after 5 measurements.

Step 4) By judging the position intervals of a ^* and b ^* in the coordinate system, it is judged whether the variety of the material to be inspected is qualified through processing.

Among them, in the CIEL*a*b* color space system, a* and b* represent different hue directions, a* represents the red and green direction, +a* represents the red direction, -a* represents the green direction; b* represents the yellow and blue direction , +b* represents the yellow direction, -b* represents the blue direction; L* represents the lightness, the larger the L*, the greater the lightness, the smaller the L*, the smaller the lightness.

Materials with b* chroma lower than 22.5 are qualified products.

The beneficial technical effects of the invention are: the chromaticity of psoraleae can easily distinguish psoralea varieties and different processing methods, and is particularly effective for identifying psoralea decoction pieces and processed products. The method has the advantages of simple operation, shortened time, low cost, feasibility and widespread popularization, and can be used as a basis for quality evaluation of the processing of Psoraleae medicinal materials.

Description of drawings

Fig. 1 The difference before and after psoralen salt roasting;

Fig. 2 The difference of ether extract and L*(D65) before and after psoralen salt-burning;

Fig. 3 The difference of ether extract and a*(D65) before and after psoralen salt-burning;

Fig. 4 The difference of ether extract and b*(D65) before and after psoralen salt-burning.

Detailed ways

Example 1

1 Preparation of psoralen samples

Psoraleae medicinal materials were collected from major Chinese medicinal material markets across the country during the national medicinal material resource census conducted by the Institute of Crude Medicine of Chongqing Institute of Traditional Chinese Medicine. There are 15 batches in total, originating from 5 origins and 13 decoction pieces factories.

The above 15 batches of medicinal materials were all identified by researcher Li Longyun (Chongqing Institute of Traditional Chinese Medicine) as the dried and ripe fruits of the leguminous plant Psoralea corylifolia Linn. In the above-mentioned dosage of auxiliary materials in the processing technology, the amount of salt used in 100kg of Psoraleae is 2kg; See Table 1 for sample information.

Table 1 Psoralea sample information table

Take 2-5 g of the test product (passed through a No. 4 sieve), accurately weigh it, and place it in a phosphorus pentoxide desiccator for 12 hours. Add an appropriate amount of diethyl ether to a Lisoxhlet extractor, and heat to reflux for 8 unless otherwise specified. After 2 hours, take the ether solution, put it in an evaporating dish that is dried to constant weight, put it aside, evaporate the ether, and dry the residue in a phosphorus pentoxide desiccator for 18 hours, accurately weigh it, slowly heat it to 105 ° C, and heat it at 105 ° C Dry to constant weight. The weight loss is the weight of the volatile ether extract. The measurement method and results are shown in Table 2 below.

Table 2 Volatile ether extracts before and after Psoralea salt preparation

2. Investigation of HPLC method

HPLC method was used to determine the content of bakuchiol in 15 batches of Bakuchi and 15 batches of decoction pieces. The results are shown in Table 3. The chromatographic conditions are as follows: select the chromatographic column Boston Symmetrix ODS-R (250×4.6mm, 5μm), the mobile phase is acetonitrile-pure water, the flow rate is 1.0mL/min, the column temperature is 30℃, and the detection wavelength is 254nm. The bakuchiol was separated, and the adaptability of the system met the requirements.

Table 3 Bakuchiol content before and after bakuchiol salt preparation

It can be seen from Table 3 that the bakuchiol content of Bakuchiol is 331.6022-567.8895 mg/g, and the content of bakuchiol in the decoction salt is 323.8859-506.4792 mg/g.

The content of bakuchiol decreased after the processing of bakuchiol by HPLC. The most abundant component in bakuchiol was bakuchiol, so the toxicity was weakened accordingly. After processing, the active ingredients such as psoralen and isopsoralen increase (for example, psoralen is decomposed into psoralen and isopsoralen in the process of heating, etc.), so the ether extract and psoralen Determination of lipid phenol content can effectively control the quality of Psoraleae medicinal materials and decoction pieces.

3. Study on the determination method of psoralen in color

Instruments and materials: Colorimeter CM-5 (KONICAMINOLTA, Japan), Psoralea medicinal material (passed through No. 3 sieve), and fried pieces of Psoralea salt (passed through No. 3 sieve).

Measurement method: L*a*b* color system: decompose the light reflected by the object at the wavelength of 360nm-740nm, and convert it into 3 numbers L*a*b*, L*(0.00-100.00 ) represents lightness, and a* and b* represent hue. Measurement conditions: diffuse illumination (integrating sphere) method; reflected light; light source: ID65 light; observation field: 10°; color system: CIE L*a*b* color system (CIE); Scanning speed: 600nm/min; slit width: 1nm; special cuvette 12mm*10mm; measurement value: the average value after 5 measurements.

The chromaticity of 15 batches of Psoraleae medicinal materials and 15 batches of decoction pieces was measured according to the chromaticity measurement method, and the results are shown in Table 4.

Table 4 chromaticity measurement results before and after psoralen salt preparation

Among them, the average value of b* value is 21.175, and then the average value of absolute deviation of the arithmetic average of this group of data is used as the range of up and down (avedev value is 2.596), and the range is 21.175±2.596)

4. Analysis of the difference in chromaticity before and after psoralea salt-burning

Select the chromaticity a*(D65) and b*(D65) data of Psoraleae medicinal material and salt-cured Psoraleae decoction pieces, take a*(D65) as the abscissa and b*(D65) as the ordinate for graph analysis, see picture 1.

It can be seen from Figure 1 that the Psoraleae medicinal materials are clustered together and relatively concentrated in the figure, while the Psoralea salt decoction pieces are clustered together and relatively dispersed. It can be seen that there are obvious differences, and they are distributed in different regions, which shows that the chromaticity of Psoraleae medicinal material and salt-fried decoction pieces are different, and there are obvious differences.

5 Correlation analysis between chromaticity and ether extracts before and after psoralea salt-burning

The ether extracts of Psoraleae medicinal materials and salt-cured Psoraleae decoction pieces were plotted and analyzed with chromaticity L*(D65), a*(D65), b*(D65) data respectively.

Correlation between Psoralea ether extracts and chromaticity L*(D65): The ether extracts of Psoraleae medicinal material and salt-cured Psoraleae decoction pieces were plotted and analyzed with chromaticity L*(D65) data respectively. The leachate is the abscissa, and L*(D65) is the ordinate, as shown in Figure 2.

It can be seen from Figure 2 that the Psoraleae medicinal materials are clustered together in the figure, in the shape of long strips, the L*(D65) data has little change, the ether extract has changed, and the Psoralea salt-fried pieces are clustered together and relatively concentrated. In addition to the large deviation of the three salt-cured decoction pieces, it can be seen that the Psoraleae medicinal material and the salt-cured decoction piece are obviously different, and they are distributed in different regions, which shows that the ether extracts of the Psoraleae medicinal material and the salt-cured decoction piece are significantly different. The difference in degree L*(D65) is small.

Correlation between Psoralea ether extracts and chromaticity a*(D65): The ether extracts of Psoraleae medicinal material and salt-cured Psoraleae decoction pieces were plotted and analyzed with chromaticity a*(D65) data, respectively. The leachate is the abscissa, and a*(D65) is the ordinate, as shown in Figure 3.

It can be seen from Figure 3 that the Psoraleae medicinal materials are clustered together in the figure, in the shape of long strips, the data of a*(D65) has little change, and the ether extract has changed. In addition to the large deviation of the three salt-cured decoction pieces, it can be seen that the Psoraleae medicinal material and the salt-cured decoction piece are obviously different, and they are distributed in different regions, which shows that the ether extracts of the Psoraleae medicinal material and the salt-cured decoction piece are significantly different. The degree a*(D65) is less different.

Correlation between Psoralea ether extracts and chromaticity b*(D65): The ether extracts of Psoraleae medicinal material and salt-cured Psoraleae decoction pieces were plotted and analyzed with chromaticity b*(D65) data respectively. The leachate is the abscissa, and b*(D65) is the ordinate, as shown in Figure 4.

It can be seen from Figure 4 that the Psoraleae medicinal materials are clustered together in the figure and are in the shape of long strips. The b*(D65) data has little change, and the ether extract has changed. In addition to the large deviation of the three salt-cured decoction pieces, it can be seen that the Psoraleae medicinal material and the salt-cured decoction piece are obviously different, and they are distributed in different regions, which shows that the ether extracts of the Psoraleae medicinal material and the salt-cured decoction piece are significantly different. There is a difference in degree b*(D65).

Claims (5)

1. a psoralen chromaticity digitization quality control method, by chromaticity digitization method, the processing quality of psoralen is identified, it is characterized in that: comprise the following steps: 1) pulverize the Psoraleae medicinal material or decoction pieces to obtain the material to be inspected; 2) The material to be tested is placed in a cuvette, and the tristimulus values X, Y, and Z are measured by the direct reading method of the stimulus value or the spectrophotometric method; 3) Calculate the tristimulus values X, Y, and Z to give L ^* , a ^* , b ^* ; 4) Judging the quality of Psoraleae medicinal materials or decoction pieces by the positions of L ^* , a ^* , b ^* in the coordinate system. 2. psoralen chromaticity digital quality control method according to claim 1, is characterized in that: measuring condition is: diffuse illumination mode; Reflected light; Light source: ID65 light; Observation field: 10 °; L*a*b* color system; start and end wavelength: 780～360nm; scanning speed: 600nm/min; slit width: 1nm; 3. psoralen chromaticity digital quality control method according to claim 1, is characterized in that: step 4) by judging a ^* , the position interval in the coordinate system of b ^* , judge whether the material to be inspected is processed qualified. 4. psoralen chromaticity digital quality control method according to claim 2, is characterized in that: in CIEL*a*b* color space system, a* and b* represent different hue directions, and a* represent red-green direction , +a* indicates the red direction, -a* indicates the green direction; b* indicates the yellow and blue direction, +b* indicates the yellow direction, -b* indicates the blue direction; L* indicates the lightness, the greater the L*, the greater the lightness, and the L *The smaller the lightness, the smaller the lightness. 5. The psoralen chromaticity digital quality control method according to claim 3, characterized in that: the materials within the range of 18.58～23.77 are processed qualified products.

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