CN112816428B - Identification method of standard decoction of fructus gardeniae, fried fructus gardeniae and coked fructus gardeniae - Google Patents
Identification method of standard decoction of fructus gardeniae, fried fructus gardeniae and coked fructus gardeniae Download PDFInfo
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- G—PHYSICS
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Abstract
The invention discloses a method for identifying standard decoction of gardenia, fried gardenia and coked gardenia, belonging to the technical field of traditional Chinese medicine analysis and quality identification and control. In the technical scheme, based on different tannin contents in three processed product standard decoctions, the distinguishing points of the gardenia standard decoction, the fried gardenia standard decoction and the burnt gardenia standard decoction are established (the tannin content of a sample is calculated by gallic acid, namely, the tannin content in the gardenia standard decoction is less than or equal to 2.8 percent, the tannin content in the fried gardenia standard decoction is 2.8-5.0 percent, and the tannin content in the burnt gardenia standard decoction is more than or equal to 5.0 percent), and systematic tannin content research is carried out on three different processed products from the decoction pieces to the standard decoction for the first time, so that the quality control technology of subsequent gardenia prescription granules and the like is more perfect and scientific, and effective basis is provided for quality control, identification and the like of traditional Chinese medicinal materials.
Description
Technical Field
The invention relates to a method for identifying traditional Chinese medicines obtained by different processing modes, in particular to a method for identifying standard decoction of gardenia, fried gardenia and coked gardenia, belonging to the technical fields of traditional Chinese medicine analysis, quality identification and control.
Background
Fructus Gardeniae (Gardenia jasminoides Ellis), also known as fructus Gardeniae, and Bufonis venenum, is fruit of Gardenia jasminoides Ellis of Rubiaceae, and has effects in protecting liver, promoting bile flow, lowering blood pressure, tranquilizing, stopping bleeding, and relieving swelling; the traditional Chinese medicine composition is used for treating icteric hepatitis, sprain and contusion, hypertension, diabetes and other symptoms in clinic; meanwhile, the crocin aglycone can be used as a yellow dye.
The fructus Gardeniae is usually prepared from different decoction pieces such as raw fructus Gardeniae, parched fructus Gardeniae, and fructus Gardeniae Preparata in clinical application, and the description of processing degree and product properties of different specifications of fructus Gardeniae in current edition of Chinese pharmacopoeia, 88 edition of national decoction piece processing Specification, various provinces of Chinese decoction piece processing Specification, chinese medicine processing science, etc. is based on appearance color as important index, and specifically comprises: the surface of the raw product is red yellow or brownish red, the inner surface color is lighter, and the seeds are dark red or reddish yellow; the surface of the fried gardenia is yellow brown or yellow red; brown, brown or black on the surface of the fructus gardeniae, brown on the inner surface of the pericarp and brown on the surface of the seed; the surface of the gardenia charcoal product is black brown or burnt black. Therefore, the color is only evaluated manually as a unique index when the gardenia is processed at present, but in the actual production process, along with the increase of processing temperature and time, the gardenia can obviously change in smell, such as obvious burnt smell.
The gardenia standard decoction is freeze-dried powder prepared by extracting, separating, concentrating and drying the gardenia decoction pieces with water, and compared with medicinal materials and decoction pieces, the inherent morphological characteristics of the gardenia decoction pieces are lost, and corresponding active components are correspondingly changed, so that the analysis of content indicative components, appearance color indexes and the like of the medicinal materials or decoction pieces is adopted, the inherent quality of the gardenia standard decoction is difficult to comprehensively reflect, and the gardenia standard decoction, the fried gardenia standard decoction and the scorched gardenia standard decoction cannot be distinguished from the characteristics.
The decoction pieces with different cape jasmine fruits are prepared by different processing modes, and the generated medicinal effects are different, for example: raw gardenia is bitter and cold in nature, can relieve cold in nature after being fried, and mainly has the effects of purging pathogenic fire, removing toxin, promoting bile flow and eliminating jaundice, clearing heat and purging pathogenic fire, and is externally used for cooling blood and relieving swelling, and is mainly used for treating internal heat (people with deficiency-cold constitution are not suitable for taking the medicine frequently); the fried gardenia is mainly used for relieving restlessness due to fire, clearing heat, promoting urination, cooling blood, detoxifying, treating febrile illness, vexation, jaundice, dark urine, stranguria with pain, hematemesis, conjunctival congestion with swelling and pain, sore and ulcer due to fire toxin, external treatment of sprain, contusion and pain and the like; and the charred fructus Gardeniae has hemostatic effect.
In the prior art, a method for identifying a gardenia and fried gardenia prescription granule is disclosed in CN 110873776A: the aim of identifying the gardenia and the fried gardenia is achieved by observing whether the fluorescent spots at the appointed positions of the thin-layer chromatographic spectrogram are developed or not; in the prior art, a quality detection and identification method for gardenia and its products is disclosed in CN 109164178A: the method adopts high performance liquid chromatography to detect and identify, and comprises the following steps: taking a sample to be detected, adding ethanol for ultrasonic extraction, filtering, and taking a subsequent filtrate as a sample solution; taking a proper amount of a geniposide, crocin I, chlorogenic acid and genipin-1-beta-D-dragon mono-disaccharide glycoside reference substance, and adding methanol to dissolve the reference substance solution; taking a sample to be detected, detecting by adopting a high performance liquid chromatography, and establishing a reference fingerprint, wherein the sample fingerprint at least contains 6 characteristic peaks, wherein the retention time of 4 peaks is the same as that of the corresponding reference peaks, and the peak area ratio of the corresponding peak of the crocin I to the peak 5 is not more than 0.7. In the prior art, a method for controlling the processing production degree and evaluating the quality of cape jasmine fruits is disclosed in CN 111579736A: the electronic nose technology capable of accurately quantifying the odor value is utilized to collect the sensor response value changed in the processing process of the gardenia, so that the technical problem that the gardenia is lack of objectivity in the evaluation process is effectively solved, and the mode of determining the digital standard, the modeling standard and the fire discriminant function based on the odor value as an index is used for on-line control in the processing process of the gardenia decoction pieces through statistical calculation; in the prior art, an on-line control method for a gardenia processing process is disclosed in CN 104931428A: a technology capable of accurately quantifying the appearance color of traditional Chinese medicine is introduced, a direct color measurement method is adopted for the peel and kernel of each decoction piece of gardenia, the color data of each decoction piece of gardenia is quantified, and a mathematical discriminant function of gardenia is determined to be used for on-line control in the processing process of the decoction pieces of gardenia through statistical calculation.
Therefore, based on the shape of the traditional Chinese medicine standard decoction, a method capable of distinguishing the gardenia, the fried gardenia and the scorched gardenia standard decoction is urgently needed.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a method for identifying a standard decoction of gardenia, fried gardenia and coked gardenia. In the technical scheme, based on different tannin contents in three processed product standard decoctions, the distinguishing points of the gardenia standard decoction, the fried gardenia standard decoction and the burnt gardenia standard decoction are established (the tannin content of a sample is calculated by gallic acid, namely, the tannin content in the gardenia standard decoction is less than or equal to 2.8 percent, the tannin content in the fried gardenia standard decoction is 2.8-5.0 percent, and the tannin content in the burnt gardenia standard decoction is more than or equal to 5.0 percent), and systematic tannin content research is carried out on three different processed products from the decoction pieces to the standard decoction for the first time, so that the quality control technology of subsequent gardenia prescription granules and the like is more perfect and scientific, and effective basis is provided for quality control, identification and the like of traditional Chinese medicinal materials.
In order to achieve the technical purpose, the following technical scheme is provided:
a method for identifying standard decoction of fructus Gardeniae, parched fructus Gardeniae and fructus Gardeniae Preparata comprises the following steps:
A. preparation of a control solution: adding water into gallic acid reference substance to obtain solution containing 50 μg per 1 mL;
B. preparation of test solution: taking powder of a to-be-tested sample, adding water, performing ultrasonic treatment, cooling, diluting, shaking, standing, filtering, removing primary filtrate, taking subsequent filtrate, diluting, and shaking to obtain the product;
C. preparation of a standard curve: taking at least two parts of the obtained reference substance solutions respectively in a gradient distribution mode according to the concentration, adding equal volume of phosphomolybdic-tungstic acid test solution respectively, adding water to a certain volume, diluting with 29% sodium carbonate solution, shaking uniformly, standing, and measuring absorbance at 760nm wavelength by ultraviolet-visible spectrophotometry;
wherein, a blank is prepared with the corresponding solvent;
establishing a standard curve by taking absorbance as an ordinate and concentration as an abscissa;
D. measurement
Total phenols: adding the obtained test solution into the phosphomolybdic tungstic acid test solution with the same volume as that of the step C, adding water, diluting with 29% sodium carbonate solution, shaking uniformly, standing, measuring absorbance at 760nm wavelength by ultraviolet-visible spectrophotometry, obtaining the content (mug/g) of gallic acid in the test solution according to the standard curve of the step C, and calculating to obtain the total phenol content in the test solution;
non-adsorbed polyphenols: adding casein into the obtained sample solution, placing in 30deg.C water bath, maintaining temperature while shaking for 1 hr, taking out, cooling, shaking, filtering, and removing primary filtrate; adding the subsequent filtrate into the phosphomolybdic tungstic acid test solution with the same volume as that of the step C, adding water, diluting with 29% sodium carbonate solution, shaking uniformly, standing, measuring absorbance at 760nm wavelength by ultraviolet-visible spectrophotometry, obtaining the content mug/g of gallic acid in the test solution according to the standard curve in the step C, and calculating to obtain the content of non-adsorbed polyphenol in the test solution;
the content of tannins was calculated as follows:
tannin content = total phenol content-non-adsorbed polyphenol content
Gardenia standard decoction: the content of tannins in the product is less than 2.8% calculated by dry product.
Standard decoction of fried gardenia: the content of tannins in the product is 2.8-5.0% calculated by dry product.
Standard decoction of fructus Gardeniae: the content of tannins in the product is greater than 5.0% calculated by dry product.
And (3) according to the total phenol content and the non-adsorbed polyphenol content in the sample solution, obtaining the tannin content, judging the standard decoction type, and obtaining a conclusion.
Furthermore, the sample injection concentration of the gallic acid is 1.004-10.036 mug/mL.
Further, in the preparation of the reference substance solution and the sample solution, a brown measuring flask is adopted for light-shielding configuration.
For the gardenia standard decoction in the technical scheme, the gardenia is raw gardenia.
By adopting the technical scheme, the beneficial technical effects brought are as follows:
1) In the invention, based on different tannin contents in three processed material standard decoction, distinguishing points of the gardenia standard decoction, the fried gardenia standard decoction and the burnt gardenia standard decoction are established (in the gardenia standard decoction, the tannin content is less than or equal to 2.8 percent; the content of tannins in the fried gardenia standard decoction is 2.8-5.0%; in the standard decoction of the fructus gardeniae, the tannin content is more than or equal to 5.0 percent, and the system tannin content research is carried out on three different processed products from decoction pieces to the standard decoction for the first time, so that the quality control technology of the subsequent fructus gardeniae formula particles and the like is more perfect and scientific, and an effective basis is provided for the quality control, identification and the like of Chinese medicinal materials;
2) The identification method is simple to operate, has the advantages of high precision, good stability, good repeatability, high accuracy and the like, and provides effective basis for quality identification of traditional Chinese medicinal materials and the like.
Drawings
FIG. 1 is a chromatogram of the results of the specificity study in example 2;
FIG. 2 is a graph of gallic acid standard curve color in example 2.
Detailed Description
In the following, it is obvious that the embodiments described are only some embodiments of the present invention, but not all embodiments, by clearly and completely describing the technical solutions in the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the following embodiments, the instrument involved comprises:
an electronic balance: ME204E/02, MS205DU, XP26 (Metrele Tolyduo instruments Co., ltd.),
ultrasonic cleaner: cell type 1810A (Shanghai morel scientific instruments limited),
ultraviolet-visible spectrophotometry instrument: agilent Cary 60 type ultraviolet spectrophotometer;
in the following examples, the reagents involved include:
phosphomolybdic tungstic acid test solution (Beijing Hua Kecheng Fine chemical products trade Co., ltd.), anhydrous sodium carbonate (Sichuan Orett chemical reagent Co., ltd., purity not less than 99.8%), casein (Shanghai mountain Pu chemical Co., ltd.), water (ultrapure water);
in the following examples, the test articles involved include:
gardenia standard decoction batch number: SY1901007;
in the following examples, the reference substances involved include:
gallic acid (China food and drug inspection institute, batch No. 110831-201605, purity 90.8%).
Example 1
A method for identifying standard decoction of fructus Gardeniae, parched fructus Gardeniae and fructus Gardeniae Preparata comprises the following steps:
A. preparation of a control solution: dissolving gallic acid reference substance 50mg in 100mL brown measuring flask, diluting to scale with water, dissolving 5mL solution in 50mL brown measuring flask, diluting to scale with water, and shaking to obtain gallic acid reference substance solution (50 μg per 1 mL);
B. preparation of test solution: taking 0.5g of the powder of the to-be-detected sample, placing the powder into a 100mL brown measuring flask, adding 70mL of water, carrying out ultrasonic treatment for 10min, cooling, diluting with water to a scale, shaking uniformly, standing (precipitating solid matters), filtering, removing primary filtrate, taking 20mL of continuous filtrate, placing the filtrate into a 100mL brown measuring flask, diluting with water to the scale, and shaking uniformly to obtain the product;
C. preparation of a standard curve: respectively taking 0.5mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL and 5.0mL of the obtained reference substance solution, respectively placing the solutions into 25mL brown measuring flasks, respectively adding 1mL of phosphomolybdic tungstic acid test solution, respectively adding 11.5mL, 11mL, 10mL, 9mL, 8mL and 7mL of water, diluting to a scale with 29% sodium carbonate solution, shaking uniformly, standing for 30min (taking the corresponding reagent as a blank reference), and measuring absorbance at 760nm by an ultraviolet-visible spectrophotometry (generally 0401);
establishing a standard curve by taking absorbance as an ordinate and concentration as an abscissa;
D. measurement
Total phenols: 2mL of the obtained test solution is taken and placed in a 25mL brown measuring flask, 1mL of phosphomolybdic tungstic acid test solution is added, 10mL of water is added, the solution is diluted to a scale by 29 percent sodium carbonate solution, the solution is uniformly shaken and placed for 30min, the absorbance is measured at 760nm wavelength by an ultraviolet-visible spectrophotometry, the content (mug/g) of gallic acid in the test solution is obtained according to the standard curve in the step C, and the total phenol content in the test solution is obtained by calculation;
non-adsorbed polyphenols: adding 25mL of the obtained sample solution into a 100mL conical flask with a plug containing 0.6g of casein, sealing, placing in a water bath at 30 ℃ for heat preservation for 1h, shaking while heat preservation, taking out, cooling, shaking uniformly, filtering, and removing primary filtrate; 2mL of the subsequent filtrate is taken, placed in a 25mL brown measuring flask, 1mL of phosphomolybdic tungstic acid test solution is added, 10mL of water is added, and 29% sodium carbonate solution is used for dilution to scale, shaking is carried out, the mixture is placed for 30min, absorbance is measured at 760nm wavelength by an ultraviolet-visible spectrophotometry, the gallic acid content (mug/g) in the test solution is obtained according to the standard curve in the step C, and the calculated polyphenol content which is not adsorbed in the test solution is obtained;
the content of tannins was calculated as follows:
tannin content = total phenol content-non-adsorbed polyphenol content
Gardenia standard decoction: the content of tannins in the product is less than 2.8% calculated by dry product.
Standard decoction of fried gardenia: the content of tannins in the product is 2.8-5.0% calculated by dry product.
Standard decoction of fructus Gardeniae: the content of tannins in the product is greater than 5.0% calculated by dry product.
And (3) according to the total phenol content and the non-adsorbed polyphenol content in the sample solution, obtaining the tannin content, judging the standard decoction type, and obtaining a conclusion.
Example 2
Based on example 1, methodology (specificity, precision, linear relationship, stability, repeatability, intermediate precision, etc.) was examined to further illustrate the technical solution of the present invention.
1. Investigation of specificity
A method for identifying standard decoction of fructus Gardeniae, parched fructus Gardeniae and fructus Gardeniae Preparata comprises the following steps:
A. preparation of a control solution: adding water into gallic acid reference substance to obtain solution containing 50 μg per 1 mL;
B. preparation of test solution: placing 2.0g of the product into a 250mL brown measuring flask, adding 150mL of water, performing ultrasonic treatment for 20min, cooling, diluting with water to a scale, shaking uniformly, standing (precipitating solid), filtering, taking 20mL of the subsequent filtrate, placing into a 100mL volumetric flask, diluting with water to the scale, and shaking uniformly to obtain the product;
C. measurement
Total phenols: taking 2mL of the obtained sample solution, placing the sample solution into a 25mL brown measuring flask, sequentially adding 1mL of phosphomolybdic tungstic acid and 10mL of water, diluting to a scale with 29% sodium carbonate solution, shaking uniformly, standing for 30min (taking a corresponding reagent as a blank control), and detecting absorbance at 760nm wavelength by an ultraviolet-visible spectrophotometry; according to the obtained standard curve, the content (mug/g) of gallic acid in the sample solution is obtained, and the total phenol content in the sample solution is obtained through calculation;
non-adsorbed polyphenols: adding 25mL of the obtained sample solution into a 100mL conical flask containing 0.6g of casein, sealing, placing in a water bath at 30 ℃ for heat preservation for 1h, taking out, cooling, shaking uniformly, filtering, removing primary filtrate, taking 2mL of the subsequent filtrate, placing in a 25mL brown measuring flask, adding 1mL of phosphomolybdic tungstic acid test solution, adding 10mL of water, diluting to scale with 29% sodium carbonate solution, shaking uniformly, placing for 30min, measuring absorbance at 760nm wavelength by ultraviolet-visible spectrophotometry, obtaining gallic acid content (mug/g) in the sample solution according to the obtained standard curve, and calculating to obtain the non-adsorbed polyphenol content in the sample solution;
tannin content = total phenol content-non-adsorbed polyphenol content
D. Preparation of negative solution: in a 25mL brown measuring flask, adding phosphomolybdic tungstic acid 1mL and water 10mL in sequence, diluting to scale with 29% sodium carbonate solution, shaking, standing for 30min, and detecting absorbance at 760nm wavelength by ultraviolet-visible spectrophotometry to obtain the result shown in FIG. 1.
The results show that: the negative solution chromatogram has no interference to the measurement of the peak to be measured, which shows that the method has good specificity.
2. Precision investigation
The control solution was sampled six times continuously, absorbance of gallic acid was recorded, and RSD value was calculated, and the results were as shown in table 1 below.
Table 1 results of precision investigation
The results show that: in the precision investigation, the absorbance RSD value of the gallic acid is 0.7%, and the method has good sample injection precision.
3. Linear relationship investigation
Taking gallic acid reference substance 5.020mg, placing into a 100mL brown measuring flask, adding water for dissolving and diluting to scale, and shaking uniformly to obtain the final product (each 1mL contains gallic acid 50.25 μg);
respectively taking 0.5mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL, 6.0mL and 7.0mL of the reference solution, respectively placing the reference solution and the reference solution into 25mL brown measuring flasks, respectively adding 1mL of the phosphomolybdenum tungstic acid test solution, respectively adding 11.5mL, 11mL, 10mL, 9mL, 8mL, 7mL, 6mL and 5mL of water, respectively diluting the reference solution to the scale with 29% sodium carbonate solution, shaking the reference solution, standing the sample for 30min, taking the corresponding reagent as a blank, measuring absorbance at 760nm wavelength by an ultraviolet-visible spectrophotometry, taking absorbance as an ordinate Y axis and taking concentration as an abscissa X axis, and drawing a standard curve, wherein the obtained results are shown in the following table 2 and figure 2.
TABLE 2 Total phenol Standard Curve analysis results
The results show that: gallic acid concentration ranges from 1.004 to 10.036 mug/mL, and the linear relation is Y=0.0792X+0.0806, and R2=0.9987; the sample injection concentration is shown to be in good linear relation when the sample injection concentration is 1.004-10.036 mug/mL.
4. Linear relationship investigation
The absorbance of the total phenol and the non-adsorbed polyphenol in the sample solutions was measured at 0min, 10min, 30min, 60min, 90min, and 120min, respectively, using the same sample (lot: SY 1901007) solution, and the results were shown in Table 3 below.
TABLE 3 stability test results
| Sequence number | Analysis time (min) | Absorbance of total phenol | Absorbance of non-adsorbed polyphenols |
| 1 | 0 | 0.599 | 0.121 |
| 2 | 10 | 0.622 | 0.115 |
| 3 | 30 | 0.623 | 0.115 |
| 4 | 60 | 0.627 | 0.124 |
| 5 | 90 | 0.496 | 0.11 |
| 6 | 120 | 0.388 | 0.106 |
The results show that: the absorbance RSD value of the total phenol is 17.4%, and the absorbance RSD value of the non-adsorbed polyphenol is 5.8%, which shows that the stability of the test sample solution is good within 120 min.
5. Repeatability investigation
The same sample (batch No. SY 1901007) was taken in an amount of 2.0g and six parts, and the gallic acid content in the six sample solutions was calculated from the sample solution preparation method and the measurement method in example 1 by the same operator, and the results are shown in Table 4 below.
TABLE 4 results of repeatability experiments
The results show that: the RSD value of the total phenol content was 4.57% and the RSD value of the non-adsorbed polyphenol was 25.96%, indicating that the process was excellent in reproducibility.
6. Intermediate precision investigation
The same sample (lot: SY 1901007) was taken, and sample solutions were prepared by different persons (A, B) at different times (I, II) for analysis, and the gallic acid content in the sample solutions was calculated, with the results shown in Table 5 below.
TABLE 5 results of intermediate precision experiments-different personnel, different time
The results show that: the RSD value of the total polyphenol content measured by different personnel and different times is 2.52%, which shows that the method has good intermediate precision.
Example 3
Based on example 1, the content of tannins in different products of different production areas is measured in the example to further explain the technical scheme in the invention.
Firstly, selecting cape jasmine decoction pieces, stir-fried cape jasmine decoction pieces and burnt cape jasmine decoction pieces in Fujian, shanxi and Jiangxi three provinces as samples, and measuring the content of tannins in the decoction pieces, wherein the results are shown in the following table 6;
next, standard decoction pieces corresponding to cape jasmine decoction pieces, stir-fried cape jasmine decoction pieces and burnt cape jasmine decoction pieces in Fujian, shanxi and Jiangxi three provinces are selected as samples, and the content of tannins in the standard decoction pieces is measured, and the results are shown in the following table 7;
finally, through researches on decoction pieces of different production places, different processed products and standard decoction, different processed products cannot be distinguished from each other according to the content of tannins in the decoction piece stage, but after the decoction pieces are decocted with water, concentrated and freeze-dried to prepare the standard decoction, different processed products can be distinguished from each other according to the content of the tannins, and the method has general applicability.
The differences of the tannin contents of the three materials are shown in the following table 8 after the study of the multi-batch gardenia standard decoction, the fried gardenia standard decoction and the burnt gardenia standard decoction.
TABLE 6 determination of tannin content of cape jasmine fruit, fried cape jasmine fruit and burnt cape jasmine decoction pieces
TABLE 7 determination of tannin content in Gardenia jasminoides Ellis Standard decoction, gardenia jasminoides Ellis decoction, and Gardenia jasminoides Ellis decoction
Table 8 fructus Gardeniae standard decoction, parched fructus Gardeniae standard decoction and fructus Gardeniae standard decoction with different tannin contents
| Sequence number | Name of product | Tannin content limit (%) |
| 1 | Gardenia standard decoction | ≤2.8 |
| 2 | Standard decoction of fried gardenia | 2.8～5.0 |
| 3 | Standard decoction of fructus Gardeniae | ≥5.0 |
Claims (4)
1. A method for identifying standard decoction of fructus gardeniae, fried fructus gardeniae and coked fructus gardeniae is characterized by comprising the following steps:
A. preparation of a control solution: adding water into gallic acid reference substance to obtain solution containing 50 μg per 1 mL;
B. preparation of test solution: taking 0.5g of the powder of the sample to be tested, placing the powder into a 100mL brown measuring flask, adding 70mL of water, carrying out ultrasonic treatment for 10min, cooling, diluting with water to a scale, shaking uniformly, standing, filtering, removing primary filtrate, taking 20mL of subsequent filtrate, placing the filtrate into a 100mL brown measuring flask, diluting with water to the scale, and shaking uniformly to obtain the product;
C. preparation of a standard curve: respectively taking 0.5mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL and 5.0mL of the obtained reference substance solution according to a gradient distribution mode, respectively placing the reference substance solution into 25mL brown measuring bottles, respectively adding 1mL of phosphomolybdic tungstic acid test solution, respectively adding 11.5mL, 11mL, 10mL, 9mL, 8mL and 7mL of water, diluting to a scale with 29% sodium carbonate solution, shaking uniformly, standing for 30min, and measuring absorbance at 760nm wavelength by an ultraviolet-visible spectrophotometry;
establishing a standard curve by taking absorbance as an ordinate and concentration as an abscissa;
D. measurement
Total phenols: 2mL of the obtained sample solution is taken and placed in a 25mL brown measuring flask, 1mL of phosphomolybdic tungstic acid sample solution is added, 10mL of water is added, the sample solution is diluted to a scale by 29% sodium carbonate solution, the sample solution is uniformly shaken and placed for 30min, the absorbance is measured at 760nm wavelength by an ultraviolet-visible spectrophotometry, the content of gallic acid in the sample solution is obtained according to the standard curve in the step C, and the total phenol content in the sample solution is obtained by calculation;
non-adsorbed polyphenols: adding 25mL of the obtained sample solution into a 100mL conical flask with a plug containing 0.6g of casein, sealing, placing in a water bath at 30 ℃ for heat preservation for 1h, shaking while heat preservation, taking out, cooling, shaking uniformly, filtering, and removing primary filtrate; 2mL of the continuous filtrate is taken and placed in a 25mL brown measuring flask, 1mL of phosphomolybdic tungstic acid test solution is added, 10mL of water is added, the solution is diluted to scale by 29 percent sodium carbonate solution, the solution is uniformly shaken and placed for 30min, absorbance is measured at 760nm wavelength by an ultraviolet-visible spectrophotometry, the content of gallic acid in the test solution is obtained according to the standard curve in the step C, and the content of non-adsorbed polyphenol in the test solution is obtained by calculation;
and (3) according to the total phenol content and the non-adsorbed polyphenol content in the sample solution, obtaining the tannin content, judging the standard decoction type, and obtaining a conclusion.
2. The method for identifying standard decoction of fructus Gardeniae, parched fructus Gardeniae and fructus Gardeniae Preparata according to claim 1, wherein brown measuring flask is used in the preparation process of the solution in step A-D.
3. The method for identifying standard decoction of fructus Gardeniae, parched fructus Gardeniae and fructus Gardeniae Preparata according to any one of claims 1-2, wherein the sample injection concentration of the gallic acid reference substance is 1.004-10.036 μg/mL.
4. The method for identifying standard decoction of fructus Gardeniae, parched fructus Gardeniae and fructus Gardeniae coke according to any one of claims 1-2, wherein the sample to be tested is dried to obtain fructus Gardeniae standard decoction with tannin content less than 2.8%; the tannin content is 2.8-5.0%, and the fructus gardeniae is a standard decoction; the tannin content is more than 5.0%, and the fructus Gardeniae is the standard decoction of fructus Gardeniae Preparata.
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| CN101474273A (en) * | 2007-12-18 | 2009-07-08 | 北京康仁堂药业有限公司 | Stir-fried fructus gardenia dispensing granule as well as preparation method and quality control method thereof |
| CN104502290A (en) * | 2014-12-17 | 2015-04-08 | 广州白云山敬修堂药业股份有限公司 | Detection method of sarcandra glabra medicinal material |
| CN104535513A (en) * | 2014-12-17 | 2015-04-22 | 广州白云山敬修堂药业股份有限公司 | Glabrous sarcandra herb extract and detection method of preparation thereof |
| WO2017148418A1 (en) * | 2016-03-03 | 2017-09-08 | 石家庄以岭药业股份有限公司 | Method for determining component contents of chinese medicine composition |
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|---|---|---|---|---|
| CN101474273A (en) * | 2007-12-18 | 2009-07-08 | 北京康仁堂药业有限公司 | Stir-fried fructus gardenia dispensing granule as well as preparation method and quality control method thereof |
| CN104502290A (en) * | 2014-12-17 | 2015-04-08 | 广州白云山敬修堂药业股份有限公司 | Detection method of sarcandra glabra medicinal material |
| CN104535513A (en) * | 2014-12-17 | 2015-04-22 | 广州白云山敬修堂药业股份有限公司 | Glabrous sarcandra herb extract and detection method of preparation thereof |
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