CN110850021A - Quality standard detection method for rhizoma gastrodiae wall-broken decoction pieces - Google Patents
Quality standard detection method for rhizoma gastrodiae wall-broken decoction pieces Download PDFInfo
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Abstract
The invention discloses a quality standard detection method of rhizoma gastrodiae wall-broken decoction pieces, which comprises identification of the rhizoma gastrodiae wall-broken decoction pieces, particle size distribution inspection, inspection of the limit of cells which are not wall-broken, appearance uniformity inspection, characteristic spectrum determination and content determination. The invention provides a systematic and scientific quality standard detection method for rhizoma gastrodiae wall-broken decoction pieces, which comprises the steps of identifying the types of the rhizoma gastrodiae wall-broken decoction pieces, checking various physical and chemical indexes and measuring pharmacological components, wherein the measurement method uses accurate control of parameters and can completely reflect the quality of the rhizoma gastrodiae wall-broken decoction pieces.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to a quality standard detection method for rhizoma gastrodiae wall-broken decoction pieces.
Background
Rhizoma Gastrodiae is dry tuber of Gastrodia elata Bl of Orchidaceae, has sweet and neutral taste, enters liver meridian, has effects of calming endogenous wind and relieving spasm, suppressing liver yang, dispelling pathogenic wind and dredging collaterals, and is used for treating infantile convulsion, epilepsia tetany, tetanus, headache giddiness, limb paralysis, limb numbness, and rheumatalgia. With the development of production technology, the traditional medicine form is changed, and the wall-broken decoction pieces are gradually entering the consumer market.
The rhizoma Gastrodiae wall-broken decoction pieces are prepared by pulverizing cell wall of traditional rhizoma Gastrodiae decoction pieces into particle size distribution D by modern superfine pulverizing technology90Making the fine particles with the particle size less than 45 mu m into particles with 30-100 meshes. Compared with the traditional decoction pieces, the decoction pieces have the characteristics of consistent color, uniform quality and good stability. Because the rhizoma gastrodiae wall-broken decoction pieces do not have the morphological characteristics of the traditional rhizoma gastrodiae decoction pieces, dissolution rate change of chemical components such as effective components or index components can be brought after wall breaking, so that the identification and quality detection methods of the traditional decoction pieces cannot be completely applicable. Therefore, a detection method which has strong specificity and can comprehensively reflect the quality condition of the rhizoma gastrodiae wall-broken decoction pieces must be established for the rhizoma gastrodiae wall-broken decoction pieces. However, it is not easy to establish a new quality detection method, and for example, the detection conditions, the selection of reference substances, and the preparation method of test samples need to be considered and verified. Although the prior art relates to a detection method of a fingerprint of a gastrodia elata traditional Chinese medicine, no method for detecting a special-shaped gastrodia elata wall-broken decoction piece exists, and the defects of specificity, stability, reproducibility and poor precision exist, and the quality condition of the decoction piece cannot be completely reflected.
Disclosure of Invention
The invention aims to make up the defects of the prior art and provides a quality standard detection method for gastrodia elata wall-broken decoction pieces.
In order to achieve the above object, the present invention provides the following technical solutions:
a quality standard detection method for rhizoma Gastrodiae wall-broken decoction pieces comprises identification of rhizoma Gastrodiae wall-broken decoction pieces, particle size distribution inspection, inspection of cell limit of non-broken wall, appearance uniformity inspection, characteristic spectrum measurement, and content measurement.
The quality standard detection method of the rhizoma gastrodiae wall-broken decoction pieces comprises the following steps of: pulverizing rhizoma Gastrodiae into fine powder, micronizing the fine powder to obtain wall-broken powder, mixing, adding ethanol with appropriate concentration, granulating, and drying to obtain granule with yellowish white to yellowish brown color, slight smell, and sweet taste.
The identification of the rhizoma gastrodiae wall-broken decoction pieces comprises the following steps:
(1) taking 0.5G of decoction piece powder, grinding, adding 5ml of 70% methanol, carrying out ultrasonic treatment for 30 minutes, filtering, taking filtrate as a test solution, taking 0.5G of a rhizoma gastrodiae reference material, preparing a reference medicinal material solution by the same method, taking a gastrodin reference substance, adding methanol to prepare a solution containing 1mg in each 1ml, taking the solution as a reference solution, carrying out a thin-layer chromatography test, sucking 10 mu l of the test solution, 5 mu l of each of the reference medicinal material solution and the reference solution, respectively dropping the solutions on the same silica gel G thin-layer plate, and mixing the solutions in a volume ratio of ethyl acetate-methanol-water of 9: 1: 0.2 of the mixed solution is used as a developing agent, the mixture is developed, taken out, dried, sprayed with 10% phosphomolybdic acid ethanol solution, and heated at 105 ℃ until the spots are clearly developed, wherein in the chromatogram of the test sample, spots with the same color should be developed at the positions corresponding to the chromatograms of the reference medicine and the reference substance;
(2) taking a p-hydroxybenzyl alcohol reference substance, adding ethanol to prepare a solution containing 1mg per 1ml, taking the solution as a reference substance solution, performing a thin-layer chromatography test, sucking 10 mu l of the sample solution, 5 mu l of the reference medicinal material solution and 5 mu l of the reference substance solution in the step 1, respectively dropping the solution on the same silica gel G thin-layer plate, and mixing the solution with petroleum ether-ethyl acetate according to a volume ratio of 1: 1, mixing the components to form a developing agent, developing, taking out, airing, spraying 10% phosphomolybdic acid ethanol solution, heating at 105 ℃ until spots are clearly developed, wherein spots with the same color should be displayed in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference drug and the reference solution.
Further, the temperature of the petroleum ether in the step 2 is 60-90 ℃.
The method for checking the particle size distribution comprises the following steps: adding appropriate amount of sample into circulation tank, opening ultrasonic switch to disperse the particles into ultramicro powder suspended in water, stopping adding sample when the light shielding rate in the test window reaches 10 + -5%, performing ultrasonic treatment for 15 min, determining powder particle diameter with laser particle size analyzer, and measuring D90Not more than 100 μm.
The method for checking the limit of the cells without broken walls comprises the following steps: weighing 0.01g of decoction pieces, adding chloral hydrate test solution-water according to the volume ratio of 1: 1, ultrasonic treatment to completely dissolve, sucking all the solutions to prepare slices, wherein each slice has the particle distribution uniformity degree without overflow and bubbles, and the number of particles of the complete cells is not more than 100 when the slice is inspected under a 100-fold microscope, for example, a plurality of complete cells are connected into a slice, and the whole slice is also more than 100 μm, and the whole slice is taken as one particle.
The method for inspecting the appearance uniformity comprises the following steps: taking appropriate amount of the beverage tablet, placing on smooth paper, and spreading for 4-6cm2The surface of the product is flattened, and the product is observed in bright places, and has uniform color and no decorative patterns or color spots.
The characteristic map determination comprises the following steps:
(1) preparation of reference solutions: taking 1g of rhizoma gastrodiae as a reference medicinal material, placing the rhizoma gastrodiae into a conical flask with a plug, precisely adding 50ml of dilute ethanol, weighing, carrying out ultrasonic treatment for 30 minutes under the conditions of 120W and 40KHz, cooling, weighing again, complementing the lost weight with the dilute ethanol, filtering, precisely taking 10ml of subsequent filtrate, concentrating until the filtrate is nearly dry and has no alcohol smell, and adding the residue with the volume ratio of 3: 97, transferring to a 25ml measuring flask, diluting to scale with the acetonitrile-water mixed solution, shaking, filtering, collecting the filtrate to obtain reference solution of reference medicinal material, collecting gastrodin reference, and adding into a container at volume ratio of 3: 97 acetonitrile-water mixed solution is prepared into solution containing 50 mug of gastrodin per 1ml, and the solution is used as reference substance solution of a reference substance;
(2) preparation of a test solution: taking 2g of decoction piece powder, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of dilute ethanol, weighing, carrying out ultrasonic treatment for 30 minutes under the conditions of 120W and 40KHz, cooling, weighing again, complementing the lost weight with dilute ethanol, filtering, precisely weighing 10ml of subsequent filtrate, concentrating until the filtrate is nearly dry and has no alcohol smell, and adding the residue with the volume ratio of 3: 97, transferring to a 25ml measuring flask, diluting to scale with the acetonitrile-water mixed solution, shaking, filtering, and collecting the filtrate;
(3) precisely sucking 10 μ l of reference solution and sample solution respectively, injecting into a liquid chromatograph, eluting with octadecylsilane chemically bonded silica as filler, acetonitrile as mobile phase A, and 0.05% phosphoric acid solution as mobile phase B according to the following gradient with detection wavelength of 220 nm;
| time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0-20 | 3 | 97 |
| 20-23 | 3→10 | 97→90 |
| 23-38 | 10→20 | 90→80 |
| 38-55 | 20→28 | 80→72 |
| 55-70 | 28→3 | 72→97 |
The number of theoretical plates is not less than 5000 calculated according to gastrodin peak, 5 characteristic peaks should be present in the sample characteristic chromatogram, and correspond to 5 characteristic peaks in the reference substance chromatogram peak of the reference medicinal material, wherein peak 1 should be consistent with the retention time of the reference substance peak of the reference substance.
The content determination comprises the following steps:
(1) preparation of control solutions: precisely weighing a gastrodin reference substance and a proper amount of a p-hydroxybenzyl alcohol reference substance, wherein the volume ratio of the reference substance to the p-hydroxybenzyl alcohol reference substance is 3: 97 acetonitrile-water mixed solution is prepared into mixed solution containing 50 mu g of gastrodin and 25 mu g of p-hydroxybenzyl alcohol per 1 ml;
(2) preparation of a test solution: taking 2g of decoction piece powder, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of dilute ethanol, weighing, carrying out ultrasonic treatment for 30 minutes under the conditions of 120W and 40KHz, cooling, weighing again, complementing the lost weight with dilute ethanol, filtering, precisely weighing 10ml of subsequent filtrate, concentrating until the filtrate is nearly dry and has no alcohol smell, and adding the residue with the volume ratio of 3: 97, transferring to a 25ml measuring flask, diluting to scale with the acetonitrile-water mixed solution, shaking, filtering, and collecting the filtrate;
(3) respectively and precisely sucking 5 mul of reference solution and sample solution, injecting into a liquid chromatograph, taking octadecylsilane chemically bonded silica as a filler, and mixing the reference solution and the sample solution according to a volume ratio of 3: 97 acetonitrile-0.05% phosphoric acid mixed solution is mobile phase, detection wavelength is 220nm, and determination of theoretical plate number should be no less than 5000 calculated according to gastrodin peak, and contains gastrodin (C)13H18O7) And p-hydroxybenzyl alcohol (C)7H8O2) The total amount of (A) should not be less than 0.25%.
Further, the quality standard detection method of the rhizoma gastrodiae wall-broken decoction pieces further comprises the following steps:
and (3) checking the granularity: the total of the sieve number I and the sieve number V cannot be passed by the granularity determination method (the second method of 0982 of the four-part general rule of the Chinese pharmacopoeia 2015 edition, the double sieving method) and the total of the sieve number I and the sieve number V cannot be passed by 15%.
And (3) moisture inspection: not more than 8.0% (the second method 0832 in the four kingdoms of the pharmacopoeia 2015 edition).
And (3) total ash content inspection: not more than 4.5% (the four-part general rule 2302 of the Chinese pharmacopoeia 2015 edition).
And (3) checking the residual quantity of sulfur dioxide: the sulfur dioxide content is measured according to a sulfur dioxide residue measuring method (2331 of the four-part general regulations in the Chinese pharmacopoeia 2015 edition), and the sulfur dioxide content is not more than 400 mg/kg.
And (3) microbial limit inspection: the granule microbial limit examination (0104 in the four-part general rule of the Chinese pharmacopoeia 2015) should meet the regulations.
Checking the loading (loading difference): it should meet the related regulations of granule (the national pharmacopoeia 2015 year edition, 0104 in the general rules of the four departments).
And (3) extract determination: the content of ethanol is not less than 15% by hot dipping method under alcohol solution extract determination (2201 in the four parts of pharmacopoeia 2015), using diluted ethanol as solvent.
The invention has the advantages that:
the invention provides a systematic and scientific quality standard detection method for rhizoma gastrodiae wall-broken decoction pieces, which comprises the steps of identifying the types of the rhizoma gastrodiae wall-broken decoction pieces, checking various physical and chemical indexes and measuring pharmacological components, wherein the measurement method uses accurate control of parameters and can completely reflect the quality of the rhizoma gastrodiae wall-broken decoction pieces.
Drawings
Fig. 1 is a characteristic spectrum determination chart of rhizoma gastrodiae wall-broken decoction pieces, wherein peak 1 is gastrodin.
Detailed Description
The technical scheme of the invention is further explained by combining the specific examples as follows:
a quality standard detection method for rhizoma Gastrodiae wall-broken decoction pieces comprises identification of rhizoma Gastrodiae wall-broken decoction pieces, particle size distribution inspection, inspection of cell limit of non-broken wall, appearance uniformity inspection, characteristic spectrum measurement, and content measurement.
The quality standard detection method of the rhizoma gastrodiae wall-broken decoction pieces comprises the following steps of: pulverizing rhizoma Gastrodiae into fine powder, micronizing the fine powder to obtain wall-broken powder, mixing, adding ethanol with appropriate concentration, granulating, and drying to obtain granule with yellowish white to yellowish brown color, slight smell, and sweet taste.
The identification of the rhizoma gastrodiae wall-broken decoction pieces comprises the following steps:
(1) taking 0.5G of decoction piece powder, grinding, adding 5ml of 70% methanol, carrying out ultrasonic treatment for 30 minutes, filtering, taking filtrate as a test solution, taking 0.5G of a rhizoma gastrodiae reference material, preparing a reference medicinal material solution by the same method, taking a gastrodin reference substance, adding methanol to prepare a solution containing 1mg in each 1ml, taking the solution as a reference solution, carrying out a thin-layer chromatography test, sucking 10 mu l of the test solution, 5 mu l of each of the reference medicinal material solution and the reference solution, respectively dropping the solutions on the same silica gel G thin-layer plate, and mixing the solutions in a volume ratio of ethyl acetate-methanol-water of 9: 1: 0.2 of the mixed solution is used as a developing agent, the mixture is developed, taken out, dried, sprayed with 10% phosphomolybdic acid ethanol solution, and heated at 105 ℃ until the spots are clearly developed, wherein in the chromatogram of the test sample, spots with the same color are displayed at the positions corresponding to the chromatograms of the reference medicine and the reference substance;
(2) taking a p-hydroxybenzyl alcohol reference substance, adding ethanol to prepare a solution containing 1mg per 1ml, taking the solution as a reference substance solution, performing a thin-layer chromatography test, sucking 10 mu l of the sample solution, 5 mu l of the reference medicinal material solution and 5 mu l of the reference substance solution in the step 1, respectively dropping the solution on the same silica gel G thin-layer plate, and mixing the solution with petroleum ether-ethyl acetate at 75 ℃ according to a volume ratio of 1: 1, mixing the components to form a developing agent, developing, taking out, airing, spraying 10% phosphomolybdic acid ethanol solution, heating at 105 ℃ until spots are clearly developed, wherein spots with the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference drug and the reference solution.
The method for checking the particle size distribution comprises the following steps: adding appropriate amount of sample into circulation tank, opening ultrasonic switch to disperse the particles into ultramicro powder suspended in water, stopping adding sample when the light shielding rate in test window reaches 10%, performing ultrasonic treatment for 15 min, and determining powder particle diameter with laser particle size analyzer D90Not more than 100 μm.
The method for checking the limit of the cells without broken walls comprises the following steps: weighing 0.01g of decoction pieces, adding chloral hydrate test solution-water according to the volume ratio of 1: 1, performing ultrasonic treatment to completely dissolve, sucking all solutions to prepare slices, wherein each slice has the characteristics of no overflow, no bubbles and uniform particle distribution, and the number of particles of the complete cells is not more than 100 when the slices are inspected under a 100-fold microscope.
The method for inspecting the appearance uniformity comprises the following steps: taking appropriate amount of the beverage, placing on smooth paper, and spreading for 5cm2The surface of the product is flattened, and the product is observed in bright places, and has uniform color and no decorative patterns or color spots.
The characteristic map determination comprises the following steps:
(1) preparation of reference solutions: taking 1g of rhizoma gastrodiae as a reference medicinal material, placing the rhizoma gastrodiae into a conical flask with a plug, precisely adding 50ml of dilute ethanol, weighing, carrying out ultrasonic treatment for 30 minutes under the conditions of 120W and 40KHz, cooling, weighing again, complementing the lost weight with the dilute ethanol, filtering, precisely taking 10ml of subsequent filtrate, concentrating until the filtrate is nearly dry and has no alcohol smell, and adding the residue with the volume ratio of 3: 97, transferring to a 25ml measuring flask, diluting to scale with the acetonitrile-water mixed solution, shaking, filtering, collecting the filtrate to obtain reference solution of reference medicinal material, collecting gastrodin reference, and adding into a container at volume ratio of 3: 97 acetonitrile-water mixed solution is prepared into solution containing 50 mug of gastrodin per 1ml, and the solution is used as reference substance solution of a reference substance;
(2) preparation of a test solution: taking 2g of decoction piece powder, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of dilute ethanol, weighing, carrying out ultrasonic treatment for 30 minutes under the conditions of 120W and 40KHz, cooling, weighing again, complementing the lost weight with dilute ethanol, filtering, precisely weighing 10ml of subsequent filtrate, concentrating until the filtrate is nearly dry and has no alcohol smell, and adding the residue with the volume ratio of 3: 97, transferring to a 25ml measuring flask, diluting to scale with the acetonitrile-water mixed solution, shaking, filtering, and collecting the filtrate;
(3) precisely sucking 10 μ l of reference solution and sample solution respectively, injecting into a liquid chromatograph, eluting with octadecylsilane chemically bonded silica as filler, acetonitrile as mobile phase A, and 0.05% phosphoric acid solution as mobile phase B according to the following gradient with detection wavelength of 220 nm;
| time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0-20 | 3 | 97 |
| 20-23 | 3→10 | 97→90 |
| 23-38 | 10→20 | 90→80 |
| 38-55 | 20→28 | 80→72 |
| 55-70 | 28→3 | 72→97 |
The number of theoretical plates is not less than 5000 according to gastrodin peak, 5 characteristic peaks are shown in the sample characteristic chromatogram, as shown in FIG. 1, and correspond to 5 characteristic peaks in the reference substance chromatogram peak of the reference medicinal material, wherein the retention time of peak 1 is consistent with that of the reference substance peak of the reference substance.
The content determination comprises the following steps:
(1) preparation of control solutions: precisely weighing a gastrodin reference substance and a proper amount of a p-hydroxybenzyl alcohol reference substance, wherein the volume ratio of the reference substance to the p-hydroxybenzyl alcohol reference substance is 3: 97 acetonitrile-water mixed solution is prepared into mixed solution containing 50 mu g of gastrodin and 25 mu g of p-hydroxybenzyl alcohol per 1 ml;
(2) preparation of a test solution: taking 2g of decoction piece powder, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of dilute ethanol, weighing, carrying out ultrasonic treatment for 30 minutes under the conditions of 120W and 40KHz, cooling, weighing again, complementing the lost weight with dilute ethanol, filtering, precisely weighing 10ml of subsequent filtrate, concentrating until the filtrate is nearly dry and has no alcohol smell, and adding the residue with the volume ratio of 3: 97, transferring to a 25ml measuring flask, diluting to scale with the acetonitrile-water mixed solution, shaking, filtering, and collecting the filtrate;
(3) respectively and precisely sucking 5 mul of reference solution and sample solution, injecting into a liquid chromatograph, taking octadecylsilane chemically bonded silica as a filler, and mixing the reference solution and the sample solution according to a volume ratio of 3: 97 acetonitrile-0.05% phosphoric acid mixed solution as mobile phase, detecting wavelength of 220nm, determining number of theoretical plates not less than 5000 calculated according to gastrodin peak, and containing gastrodin (C)13H18O7) And p-hydroxybenzyl alcohol (C)7H8O2) The total amount of the components is not less than 0.25%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A quality standard detection method for rhizoma Gastrodiae wall-broken decoction pieces is characterized by comprising identification of rhizoma Gastrodiae wall-broken decoction pieces, particle size distribution inspection, inspection of cell limit of non-broken wall, appearance uniformity inspection, characteristic spectrum determination, and content determination.
2. The quality standard detection method of rhizoma gastrodiae wall-broken decoction pieces according to claim 1, wherein the rhizoma gastrodiae wall-broken decoction pieces are wall-broken decoction pieces prepared by processing dried tubers of rhizoma gastrodiae of the family orchidaceae.
3. The quality standard detection method of the rhizoma gastrodiae wall-broken decoction pieces as claimed in claim 1, wherein the identification of the rhizoma gastrodiae wall-broken decoction pieces comprises the following steps:
(1) taking 0.5G of decoction piece powder, grinding, adding 5ml of 70% methanol, carrying out ultrasonic treatment for 30 minutes, filtering, taking filtrate as a test solution, taking 0.5G of a rhizoma gastrodiae reference material, preparing a reference medicinal material solution by the same method, taking a gastrodin reference substance, adding methanol to prepare a solution containing 1mg in each 1ml, taking the solution as a reference solution, carrying out a thin-layer chromatography test, sucking 10 mu l of the test solution, 5 mu l of each of the reference medicinal material solution and the reference solution, respectively dropping the solutions on the same silica gel G thin-layer plate, and mixing the solutions in a volume ratio of ethyl acetate-methanol-water of 9: 1: 0.2 of the mixed solution is used as a developing agent, the mixture is developed, taken out, dried, sprayed with 10% phosphomolybdic acid ethanol solution, and heated at 105 ℃ until the spots are clearly developed, wherein in the chromatogram of the test sample, spots with the same color should be developed at the positions corresponding to the chromatograms of the reference medicine and the reference substance;
(2) taking a p-hydroxybenzyl alcohol reference substance, adding ethanol to prepare a solution containing 1mg per 1ml, taking the solution as a reference substance solution, performing a thin-layer chromatography test, sucking 10 mu l of the sample solution, 5 mu l of the reference medicinal material solution and 5 mu l of the reference substance solution in the step 1, respectively dropping the solution on the same silica gel G thin-layer plate, and mixing the solution with petroleum ether-ethyl acetate according to a volume ratio of 1: 1, mixing the components to form a developing agent, developing, taking out, airing, spraying 10% phosphomolybdic acid ethanol solution, heating at 105 ℃ until spots are clearly developed, wherein spots with the same color should be displayed in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference drug and the reference solution.
4. The quality standard detection method of rhizoma gastrodiae wall-broken decoction pieces according to claim 3, characterized in that the temperature of petroleum ether in step 2 is 60-90 ℃.
5. The quality standard detection method of rhizoma gastrodiae wall-broken decoction pieces according to claim 1, wherein the method for checking the particle size distribution comprises the following steps: adding appropriate amount of sample into circulation tank, opening ultrasonic switch to disperse the particles into ultramicro powder suspended in water, stopping adding sample when the light shielding rate in the test window reaches 10 + -5%, performing ultrasonic treatment for 15 min, determining powder particle diameter with laser particle size analyzer, and measuring D90Not more than 100 μm.
6. The quality standard detection method of rhizoma gastrodiae wall-broken decoction pieces according to claim 1, wherein the method for checking the limit of cells that are not wall-broken is as follows: weighing 0.01g of decoction pieces, adding chloral hydrate test solution-water according to the volume ratio of 1: 1, ultrasonic treatment to completely dissolve, sucking all the solutions to prepare slices, wherein each slice has the particle distribution uniformity degree without overflow and bubbles, and the number of particles of the complete cells is not more than 100 when the slice is inspected under a 100-fold microscope, for example, a plurality of complete cells are connected into a slice, and the whole slice is also more than 100 μm, and the whole slice is taken as one particle.
7. The quality standard detection method of the rhizoma gastrodiae wall-broken decoction pieces as claimed in claim 1, wherein the method for detecting the uniformity of appearance comprises the following steps: taking appropriate amount of the beverage tablet, placing on smooth paper, and spreading for 4-6cm2The surface of the product is flattened, and the product is observed in bright places, and has uniform color and no decorative patterns or color spots.
8. The quality standard detection method of the rhizoma gastrodiae wall-broken decoction pieces as claimed in claim 1, wherein the characteristic spectrum determination comprises the following steps:
(1) preparation of reference solutions: taking 1g of rhizoma gastrodiae as a reference medicinal material, placing the rhizoma gastrodiae into a conical flask with a plug, precisely adding 50ml of dilute ethanol, weighing, carrying out ultrasonic treatment for 30 minutes under the conditions of 120W and 40KHz, cooling, weighing again, complementing the lost weight with the dilute ethanol, filtering, precisely taking 10ml of subsequent filtrate, concentrating until the filtrate is nearly dry and has no alcohol smell, and adding the residue with the volume ratio of 3: 97, transferring to a 25ml measuring flask, diluting to scale with the acetonitrile-water mixed solution, shaking, filtering, collecting the filtrate to obtain reference solution of reference medicinal material, collecting gastrodin reference, and adding into a container at volume ratio of 3: 97 acetonitrile-water mixed solution is prepared into solution containing 50 mug of gastrodin per 1ml, and the solution is used as reference substance solution of a reference substance;
(2) preparation of a test solution: taking 2g of decoction piece powder, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of dilute ethanol, weighing, carrying out ultrasonic treatment for 30 minutes under the conditions of 120W and 40KHz, cooling, weighing again, complementing the lost weight with dilute ethanol, filtering, precisely weighing 10ml of subsequent filtrate, concentrating until the filtrate is nearly dry and has no alcohol smell, and adding the residue with the volume ratio of 3: 97, transferring to a 25ml measuring flask, diluting to scale with the acetonitrile-water mixed solution, shaking, filtering, and collecting the filtrate;
(3) precisely sucking 10 μ l of reference solution and sample solution respectively, injecting into a liquid chromatograph, eluting with octadecylsilane chemically bonded silica as filler, acetonitrile as mobile phase A, and 0.05% phosphoric acid solution as mobile phase B according to the following gradient with detection wavelength of 220 nm;
The number of theoretical plates is not less than 5000 calculated according to gastrodin peak, 5 characteristic peaks should be present in the sample characteristic chromatogram, and correspond to 5 characteristic peaks in the reference substance chromatogram peak of the reference medicinal material, wherein peak 1 should be consistent with the retention time of the reference substance peak of the reference substance.
9. The quality standard detection method of the rhizoma gastrodiae wall-broken decoction pieces as claimed in claim 1, wherein the content determination comprises the following steps:
(1) preparation of control solutions: precisely weighing a gastrodin reference substance and a proper amount of a p-hydroxybenzyl alcohol reference substance, wherein the volume ratio of the reference substance to the p-hydroxybenzyl alcohol reference substance is 3: 97 acetonitrile-water mixed solution is prepared into mixed solution containing 50 mu g of gastrodin and 25 mu g of p-hydroxybenzyl alcohol per 1 ml;
(2) preparation of a test solution: taking 2g of decoction piece powder, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of dilute ethanol, weighing, carrying out ultrasonic treatment for 30 minutes under the conditions of 120W and 40KHz, cooling, weighing again, complementing the lost weight with dilute ethanol, filtering, precisely weighing 10ml of subsequent filtrate, concentrating until the filtrate is nearly dry and has no alcohol smell, and adding the residue with the volume ratio of 3: 97, transferring to a 25ml measuring flask, diluting to scale with the acetonitrile-water mixed solution, shaking, filtering, and collecting the filtrate;
(3) respectively and precisely sucking 5 mul of reference solution and sample solution, injecting into a liquid chromatograph, taking octadecylsilane chemically bonded silica as a filler, and mixing the reference solution and the sample solution according to a volume ratio of 3: 97 acetonitrile-0.05% phosphoric acid mixed solution is mobile phase, detection wavelength is 220nm, the number of theoretical plates is determined to be not less than 5000 according to gastrodin peak, and the total amount of gastrodin and p-hydroxybenzyl alcohol is not less than 0.25%.
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