CN115032316A - Quality evaluation method of Gaodanling tablets - Google Patents
Quality evaluation method of Gaodanling tablets Download PDFInfo
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- 238000013441 quality evaluation Methods 0.000 title claims abstract description 17
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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Abstract
A quality evaluation method of Gaodaoling tablet belongs to the technical field of quality evaluation of compound Chinese medicinal preparation, and comprises grinding Gaodaoling tablet, adding methanol, ultrasonic extracting, and filtering with filter membrane; precisely weighing a reference substance and adding methanol to prepare a reference substance solution with a certain concentration; acetonitrile-potassium dihydrogen phosphate solution is selected as a mobile phase, and gradient elution is adopted; the detector is selected from DAD, and the chromatographic column is selected from BEH C 18 (ii) a Measuring to obtain 10 batches of sample HPLC (high performance liquid chromatography) spectrums, introducing the obtained HPLC spectrums into similarity evaluation software, calculating sample similarity, and determining standard fingerprint spectrums; if the similarity is more than 0.90, the quality requirement of the Gaoluoling tablets is met, and thus the quality evaluation of the Gaoluoling tablet samples to be detected is completed. The invention utilizes the ultra-high performance liquid chromatography to construct the fingerprint of the GaoDouling tablet, analyzes a plurality of batches of GaoDouling tablets to determine the standard fingerprint,and a stable and reliable quality evaluation method of the liver bean tablets is established.
Description
Technical Field
The invention belongs to the technical field of quality evaluation of compound traditional Chinese medicine preparations, and particularly relates to a quality evaluation method of Ganduoling tablets.
Background
At present, the fingerprint spectrum technology of traditional Chinese medicine mainly comprises thin layer scanning (TLCS), High Performance Liquid Chromatography (HPLC), Gas Chromatography (GC), High Performance Capillary Electrophoresis (HPCE) and other chromatography methods, and ultraviolet spectroscopy (UV), infrared spectroscopy (IR), Mass Spectrometry (MS), Nuclear Magnetic Resonance (NMR) and X-ray diffraction method and other spectroscopy methods.
Because High Performance Liquid Chromatography (HPLC) has the characteristics of high separation efficiency, high selectivity, high detection sensitivity, high analysis speed, wide application range and the like, most of the traditional Chinese medicine components can be analyzed and detected on a high performance liquid chromatograph. Therefore, the high performance liquid chromatography has become the first choice of the traditional Chinese medicine fingerprint spectrum technology.
The Gaoluoling tablet is a hospital preparation in the first subsidiary hospital of Anhui Chinese medicinal university. The prescription of the preparation mainly comprises Chinese medicines such as coptis chinensis, salvia miltiorrhiza and the like, and has the main effects of clearing away heat and toxic materials, removing blood stasis and softening hard masses, and benefiting gallbladder and removing copper. At present, the main quality control method of the preparation is to use coptis chinensis in the preparation as a reference medicinal material and determine the content of berberine hydrochloride and aloe-emodin in the preparation by an HPLC method. However, the existing quality control method has a single means and cannot comprehensively control and reflect the quality of the preparation.
Disclosure of Invention
In order to solve the technical problems, the invention provides a quality evaluation method of Ganduoling tablets, which adopts HPLC technology to firstly establish fingerprint spectra of Ganduoling tablets and then realize more comprehensive control of the quality of the preparation.
The technical scheme adopted by the invention is as follows: a quality evaluation method of Gaodanling tablets comprises the following steps:
(1) preparation of Ganduoling tablet
The prescription of the Gaodaoling tablet comprises the following components: 182g of coptis root, 91g of salvia miltiorrhiza, 91g of suberect spatholobus stem, 82g of rhubarb, 82g of zedoary and 82g of turmeric;
the production method of the liver bean tablet comprises the following steps:
mixing and spreading rhubarb, zedoary and turmeric in a baking pan, putting the mixture into the baking pan for drying (less than or equal to 75 ℃), crushing the mixture, and sieving the crushed mixture with a 100-mesh sieve to obtain fine powder for later use;
② coarse powder, coptis root and salvia miltiorrhiza are mixed and extracted twice by 75 percent ethanol, 10 times of ethanol is added for 2 hours of reflux for the first time, 8 times of ethanol is added for 1.5 hours of reflux for the second time, and the ethanol extract is mixed, filtered and recovered; decocting the dregs of a decoction for 1 hour by adding 8 times of water, filtering, standing and precipitating for 48 hours, sucking supernatant, merging the supernatant with an alcohol extract, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃);
thirdly, adding water into the suberect spatholobus stem for decocting and extracting for three times, adding 10 times of water for decocting for 1.5 hours for the first time, adding 8 times of water for decocting for 1 hour for the second time and the third time, merging decoction, filtering, standing and precipitating for 48 hours, sucking supernatant fluid, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃);
mixing the two clear pastes, adding the fine powder of the medicine, 90g of starch and 20mL of simple syrup, granulating, drying (below 75 ℃), granulating (sieving with an upper sieve of 10 meshes and sieving with a lower sieve of 60 meshes), adding 1.5g of magnesium stearate, mixing uniformly, and pressing into 1000 tablets to obtain Gaodaoling tablets;
(2) preparation of a test solution:
taking 10 Gaodaoling tablets, grinding, taking 0.3g of fine powder, placing in a 10ml volumetric flask, adding methanol to a constant volume, carrying out ultrasonic treatment for 20 minutes, centrifuging at a rotating speed of 12000r/min, taking filtrate, and filtering with a 0.22 mu m filter membrane to obtain a test solution;
(3) preparation of a reference solution:
precisely weighing reference substances including epiberberine, coptisine, palmatine, berberine hydrochloride, aloe-emodin, rhein, tanshinone I and tanshinone IIA, adding methanol to prepare 0.239mg/ml of epiberberine, 0.211mg/ml of coptisine, 0.277mg/ml of palmatine, 0.216mg/ml of berberine hydrochloride, 0.243mg/ml of aloe-emodin, 0.252mg/ml of rhein, 0.224mg/ml of tanshinone I and 0.261mg/ml of tanshinone II;
(4) chromatographic conditions are as follows:
acetonitrile (A) -potassium dihydrogen phosphate solution (pH value is adjusted to 3.0 by phosphoric acid) (B) is selected as a mobile phase, and gradient elution is adopted; the elution conditions were: 0-2min, 22% A; 2-9min, 22% A; 9-12min, 25% A; 12-14min, 55% A; 14-22min, 65% A; 22-23min, 100% A; 23-24min, 15% A; 24-25min, 15% A; stopping after 25 min;
DAD is selected as a detector, and the detection wavelength is 250 nm; the column temperature was 30.0 ℃; the flow rate is 0.2 ml/min; the sample amount is 1 ul; selection of chromatographic column with ACQUITY UPLC BEH C 18 ；
(5) Establishing a fingerprint spectrum:
preparing 10 batches of liver bean tablet sample test solution, respectively injecting samples according to the chromatographic conditions to obtain 10 batches of sample HPLC (high performance liquid chromatography) spectrums, introducing the samples into similarity evaluation software, calculating the similarity of 10 batches of samples, and determining standard fingerprint spectrums;
injecting the prepared reference substance solution under the same chromatographic condition for analysis, comparing the obtained reference substance spectrum with the standard fingerprint spectrum, and identifying the chromatographic peak number corresponding to the reference substance in the standard fingerprint spectrum;
(6) and (3) quality evaluation:
after the fingerprint is established, methodology verification is carried out to investigate precision, stability and repeatability, the sample to be detected is detected under the same chromatographic conditions, the detection result is compared and evaluated through similarity evaluation software, and if the similarity is more than 0.90, the quality requirement of the liver bean tablet to be detected is met, so that the quality evaluation of the liver bean tablet sample to be detected is completed.
The invention provides a prescription of Gaodanling tablet and a production method thereof, wherein the prescription of Gaodanling tablet comprises the following components: 182g of coptis root, 91g of salvia miltiorrhiza, 91g of suberect spatholobus stem, 82g of rhubarb, 82g of zedoary and 82g of turmeric; the production method of the liver bean tablet comprises the following steps:
mixing and spreading rhubarb, zedoary and turmeric in a baking pan, putting the mixture into a baking oven for drying (less than or equal to 75 ℃), crushing the mixture, and sieving the crushed mixture with a 100-mesh sieve to obtain fine powder for later use;
mixing coarse powder with coptis root and salvia miltiorrhiza, performing reflux extraction twice by using 75% ethanol, adding 10 times of ethanol for refluxing for 2 hours for the first time, adding 8 times of ethanol for refluxing for 1.5 hours for the second time, mixing ethanol extract, filtering, and recovering ethanol; decocting the dregs of a decoction for 1 hour by adding 8 times of water, filtering, standing and precipitating for 48 hours, sucking supernatant, merging the supernatant with an alcohol extract, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃);
thirdly, adding water into the suberect spatholobus stem for decocting and extracting for three times, adding 10 times of water for decocting for 1.5 hours for the first time, adding 8 times of water for decocting for 1 hour for the second time and the third time, merging decoction, filtering, standing and precipitating for 48 hours, sucking supernatant fluid, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃);
mixing the two kinds of clear paste, adding the medicine fine powder, 90g of starch and 20mL of simple syrup, granulating, drying (less than 75 ℃), granulating (10 meshes on an upper sieve and 60 meshes on a lower sieve), adding 1.5g of magnesium stearate, mixing uniformly, and pressing into 1000 tablets to obtain the Gaodaoling tablets; the characteristics of the GaoDouling tablet are as follows: a yellowish brown flake; slightly fragrant smell, bitter and astringent taste.
The beneficial effects of the invention are as follows:
(1) the fingerprint technology is a comprehensive identification means, has strong specificity, high stability and good repeatability, and can comprehensively evaluate the authenticity and the excellence of the medicinal materials. Therefore, the invention constructs the fingerprint of the Ganduoling tablet by using the ultra-high performance liquid chromatography, analyzes a plurality of batches of Ganduoling tablets to determine the standard fingerprint, and establishes a stable and reliable quality control method of the Ganduoling tablet.
(2) The invention selects reasonable chromatographic conditions and chromatographic columns, and has good separation effect, high reproducibility and excellent identification effect. The verification of the method shows that the instrument precision is good, the sample stability is good, the method repeatability is good, the technical requirements of the fingerprint spectrum are met, and a better evaluation method is provided for the quality control of the liver bean tablets.
(3) The liver bean tablet provided by the invention has reasonable formula compatibility, can clear away heat and toxic materials, remove blood stasis and soften hard mass, promote bile flow and remove copper, and has a good curative effect on hepatolenticular degeneration.
Drawings
FIG. 1 shows the standard fingerprint of Ganduoling tablet.
FIG. 2 is an overlay of HPLC finger prints of 10 batches of Ganjianling tablets.
FIG. 3 is a comparison of 8 single control samples of Gaodanling tablets and their finger prints.
Detailed Description
Example 1
The invention provides a quality evaluation method of Gaodaoling tablets, which comprises the following steps:
(1) production of Ganduoling tablets:
the prescription of the Gaodaoling tablet comprises the following components: 182g of coptis root, 91g of salvia miltiorrhiza, 91g of suberect spatholobus stem, 82g of rhubarb, 82g of curcuma zedoary and 82g of turmeric; the production method of the liver bean tablet comprises the following steps:
mixing and spreading the rhubarb, the zedoary and the turmeric in a baking pan, putting the mixture into the baking pan for drying (less than or equal to 75 ℃), crushing the mixture, and sieving the crushed mixture by a 100-mesh sieve to obtain fine powder for later use.
② the coarse powder, coptis root and salvia miltiorrhiza are mixed and extracted twice by 75 percent ethanol, 10 times of ethanol is added for 2 hours of reflux for the first time, 8 times of ethanol is added for 1.5 hours of reflux for the second time, the ethanol extract is mixed, filtered and the ethanol is recovered. Decocting the medicine dregs with 8 times of water for 1 hour, filtering, standing and precipitating for 48 hours, sucking the supernatant, merging the supernatant with the alcohol extract, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃).
Thirdly, adding water into the suberect spatholobus stem to decoct and extract for three times, adding 10 times of water to decoct for 1.5 hours for the first time, adding 8 times of water to decoct for 1 hour for the second time and the third time, merging the decoction, filtering, standing and precipitating for 48 hours, absorbing supernatant, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃).
Mixing the two kinds of clear paste, adding the medicine fine powder, 90g of starch and 20mL of simple syrup, granulating, drying (less than 75 ℃), granulating (10 meshes on an upper sieve and 60 meshes on a lower sieve), adding 1.5g of magnesium stearate, mixing uniformly, and pressing into 1000 tablets to obtain the Gaodaoling tablets;
(2) preparation of a test solution:
10 batches of Ganjianling tablets were prepared as described above, with the batch numbers shown in Table 1.
TABLE 1.10 batch Ganjouling tablet batch number
Taking 10 tablets of Gaodaoling, grinding, precisely weighing about 0.3g into a volumetric flask, adding methanol to constant volume to 10ml, ultrasonically extracting for 20min, centrifuging at 12000r/min, taking filtrate, and filtering with a 0.22 μm filter membrane to obtain a test solution.
(3) Preparation of a reference solution:
the reference substances of epiberberine, coptisine, palmatine, berberine hydrochloride, aloe-emodin, rhein, tanshinone I and tanshinone IIA are precisely weighed, and are added with methanol to prepare 0.239mg/ml of epiberberine, 0.211mg/ml of coptisine, 0.277mg/ml of palmatine, 0.216mg/ml of berberine hydrochloride, 0.243mg/ml of aloe-emodin, 0.252mg/ml of rhein, 0.224mg/ml of tanshinone I and 0.261mg/ml of tanshinone II.
(4) Chromatographic conditions are as follows:
acetonitrile (A) -potassium dihydrogen phosphate solution (pH value is adjusted to 3.0 by phosphoric acid) (B) is selected as a mobile phase, and gradient elution is adopted; the elution conditions were: 0-2min, 22% A; 2-9min, 22% A; 9-12min, 25% A; 12-14min, 55% A; 14-22min, 65% A; 22-23min, 100% A; 23-24min, 15% A; 24-25min, 15% A; stop after 25 min.
DAD is selected as a detector, and the detection wavelength is 250 nm; the column temperature was 30.0 ℃; the flow rate is 0.2 ml/min; the sample injection amount is 1 mu L; selection of chromatographic column with ACQUITY UPLC BEH C 18 。
(5) Establishing a fingerprint spectrum:
and (3) respectively injecting sample solutions of 10 batches of liver bean tablet samples according to the chromatographic conditions to obtain HPLC (high performance liquid chromatography) spectrums of 10 batches of samples, and determining 19 common peaks to form a common mode. Wherein, the 11 peak is a reference peak, the relative retention time and the relative peak area are 1, the relative retention time and the relative peak area are calculated by comparing other peaks, and the result is shown in the table 2. Thereby obtaining the standard fingerprint of the GaoDouling tablet, as shown in figure 1.
TABLE 2.10 relative peak areas and relative retention times for 19 peaks of a batch of Ganguoling tablets
Note: peak 11 is a reference peak, (RRT: relative retention time, RPA: relative peak area)
The analysis results were imported into similarity evaluation software (traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2004A edition, the same below)), and the similarity was calculated by means of an averaging method to obtain similarity data of 10 batches of samples, the results are shown in table 3, and the HPLC chromatogram overlay of each sample is shown in fig. 2.
Table 310 results of similarity data for samples
The HPLC spectra and the fingerprint spectra of 8 reference substances, namely epiberberine, coptisine, palmatine, berberine hydrochloride, aloe-emodin, rhein, tanshinone I and tanshinone IIA, are combined and compared, so as to indicate that quercetin, calycosin, lobetyolin, echinacoside and verbascoside are respectively as follows in 19 common peaks: the corresponding peak numbers are peaks 8, 9, 11, 12, 13, 14, 16 and 19. The results are shown in FIG. 3.
(6) Methodology investigation
Examination of precision
Preparing an S5 sample according to the preparation method of the test solution, repeatedly injecting samples for 6 times under the determined optimal chromatographic conditions, and measuring that the relative retention time of all common peaks and the RSD value of the relative peak area are between 0.117-1.084% and 0.038-1.990% (shown in Table 4), which indicates that the precision of the instrument is good and meets the technical requirements of fingerprint spectrum.
TABLE 4 results of the precision test
Note: peak 11 is a reference peak, (RRT: relative retention time, RPA: relative peak area)
② stability test
The sample No. S5 is prepared according to the preparation method of the test solution, the determined optimal chromatographic conditions are respectively subjected to sample injection analysis for 0 hour, 4 hour, 8 hour, 12 hour, 16 hour and 24 hour, and the RSD value of the relative retention time and the relative peak area of each common peak is measured to be between 0.195-2.366 percent and 0.329-2.752 percent (shown in Table 5), which indicates that the test solution has good stability within 24 hours.
TABLE 5 stability test results
Note: peak 11 is a reference peak, (RRT: relative retention time, RPA: relative peak area)
③ repeatability test
6 samples of No. S5 are prepared in parallel according to the determined preparation method of the test solution, the determined optimal chromatographic conditions are subjected to sample injection analysis respectively, and the RSD value of the relative retention time and the relative peak area of each common peak is measured to be between 0.135-1.490% and 0.433-2.425% (shown in Table 6), which indicates that the method has good repeatability.
TABLE 6 results of repeated experiments
Note: peak 11 is a reference peak, (RRT: relative retention time, RPA: relative peak area)
(7) Evaluation of Gaodaoling tablet quality
Preparing a sample to be detected according to the preparation method of the test solution, detecting the sample to be detected by using the same chromatographic conditions, and comparing and evaluating the detection result by using similarity evaluation software, wherein the similarity of more than 0.90 meets the quality requirement of the GaoDouling tablets, thereby completing the quality evaluation of the GaoDouling tablet sample to be detected.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (2)
1. A quality evaluation method of Gaodanling tablets is characterized by comprising the following steps:
(1) preparation of Ganduoling tablet
The prescription of the Gaodaoling tablet comprises the following components: 182g of coptis root, 91g of salvia miltiorrhiza, 91g of suberect spatholobus stem, 82g of rhubarb, 82g of curcuma zedoary and 82g of turmeric;
the production method of the Ganduoling tablet comprises the following steps:
mixing and spreading rhubarb, zedoary and turmeric in a baking pan, putting the mixture into a baking oven for drying (less than or equal to 75 ℃), crushing the mixture, and sieving the crushed mixture with a 100-mesh sieve to obtain fine powder for later use;
② coarse powder, coptis root and salvia miltiorrhiza are mixed and extracted twice by 75 percent ethanol, 10 times of ethanol is added for 2 hours of reflux for the first time, 8 times of ethanol is added for 1.5 hours of reflux for the second time, and the ethanol extract is mixed, filtered and recovered; decocting the dregs of a decoction for 1 hour by adding 8 times of water, filtering, standing and precipitating for 48 hours, sucking supernatant, merging the supernatant with an alcohol extract, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃);
thirdly, adding water into the suberect spatholobus stem for decocting and extracting for three times, adding 10 times of water for decocting for 1.5 hours for the first time, adding 8 times of water for decocting for 1 hour for the second time and the third time, merging decoction, filtering, standing and precipitating for 48 hours, sucking supernatant fluid, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃);
mixing the two kinds of clear paste, adding the medicine fine powder, 90g of starch and 20mL of simple syrup, granulating, drying (less than 75 ℃), granulating (10 meshes on an upper sieve and 60 meshes on a lower sieve), adding 1.5g of magnesium stearate, mixing uniformly, and pressing into 1000 tablets to obtain the Gaodaoling tablets;
(2) preparing a test solution:
taking 10 Gaodaoling tablets, grinding, taking 0.3g of fine powder, placing in a 10ml volumetric flask, adding methanol to a constant volume, carrying out ultrasonic treatment for 20 minutes, centrifuging at a rotating speed of 12000r/min, taking filtrate, and filtering with a 0.22 mu m filter membrane to obtain a test solution;
(3) preparation of a control solution:
precisely weighing reference substances including epiberberine, coptisine, palmatine, berberine hydrochloride, aloe-emodin, rhein, tanshinone I and tanshinone IIA, adding methanol to prepare 0.239mg/ml of epiberberine, 0.211mg/ml of coptisine, 0.277mg/ml of palmatine, 0.216mg/ml of berberine hydrochloride, 0.243mg/ml of aloe-emodin, 0.252mg/ml of rhein, 0.224mg/ml of tanshinone I and 0.261mg/ml of tanshinone II;
(4) chromatographic conditions are as follows:
acetonitrile (A) -potassium dihydrogen phosphate solution (pH value is adjusted to 3.0 by phosphoric acid) (B) is selected as a mobile phase, and gradient elution is adopted; the elution conditions were: 0-2min, 22% A; 2-9min, 22% A; 9-12min, 25% A; 12-14min, 55% A; 14-22min, 65% A; 22-23min, 100% A; 23-24min, 15% A; 24-25min, 15% A; stopping after 25 min;
DAD is selected as a detector, and the detection wavelength is 250 nm; the column temperature was 30.0 ℃; the flow rate is 0.2 ml/min; the sample amount is 1 ul; selection of chromatographic column with ACQUITY UPLC BEH C 18 ；
(5) Establishing a fingerprint spectrum:
preparing 10 batches of liver bean tablet sample test solution, respectively injecting samples according to the chromatographic conditions to obtain 10 batches of sample HPLC (high performance liquid chromatography) spectrums, introducing the samples into similarity evaluation software, calculating the similarity of 10 batches of samples, and determining standard fingerprint spectrums;
injecting the prepared reference substance solution under the same chromatographic condition for analysis, comparing the obtained reference substance spectrum with the standard fingerprint spectrum, and identifying the chromatographic peak number corresponding to the reference substance in the standard fingerprint spectrum;
(6) and (3) quality evaluation:
after the fingerprint is established, methodology verification is carried out to investigate precision, stability and repeatability, the sample to be detected is detected under the same chromatographic conditions, the detection result is compared and evaluated through similarity evaluation software, and if the similarity is more than 0.90, the quality requirement of the liver bean tablet to be detected is met, so that the quality evaluation of the liver bean tablet sample to be detected is completed.
2. The production method of the liver bean tablet is characterized in that the prescription of the liver bean tablet comprises the following components: 182g of coptis root, 91g of salvia miltiorrhiza, 91g of suberect spatholobus stem, 82g of rhubarb, 82g of curcuma zedoary and 82g of turmeric; the production method of the liver bean tablet comprises the following steps:
mixing and spreading rhubarb, zedoary and turmeric in a baking pan, putting the mixture into the baking pan for drying (less than or equal to 75 ℃), crushing the mixture, and sieving the crushed mixture with a 100-mesh sieve to obtain fine powder for later use;
mixing coarse powder with coptis root and salvia miltiorrhiza, performing reflux extraction twice by using 75% ethanol, adding 10 times of ethanol for refluxing for 2 hours for the first time, adding 8 times of ethanol for refluxing for 1.5 hours for the second time, mixing ethanol extract, filtering, and recovering ethanol; decocting the dregs of a decoction for 1 hour by adding 8 times of water, filtering, standing and precipitating for 48 hours, sucking supernatant, merging the supernatant with an alcohol extract, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃);
thirdly, adding water into the suberect spatholobus stem for decocting and extracting for three times, adding 10 times of water for decocting for 1.5 hours for the first time, adding 8 times of water for decocting for 1 hour for the second time and the third time, merging decoction, filtering, standing and precipitating for 48 hours, sucking supernatant fluid, and concentrating under reduced pressure (the pressure is-0.02 to-0.04 MPa) to obtain clear paste with the relative density of 1.10(60 ℃);
mixing the two clear pastes, adding the fine powder of the medicine, 90g of starch and 20mL of simple syrup, granulating, drying (below 75 ℃), granulating (sieving with an upper sieve of 10 meshes and sieving with a lower sieve of 60 meshes), adding 1.5g of magnesium stearate, mixing uniformly, and pressing into 1000 tablets to obtain Gaodaoling tablets; the characteristics of the GaoDouling tablet are as follows: a yellowish brown flake; slightly fragrant smell, bitter and astringent taste.
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| 张雪燕: "肝豆汤质量控制及其对铜负荷HLD模型大鼠排铜保肝作用的研究", 中国优秀硕士学位论文全文数据库医药卫生科技辑, no. 3 * |
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