CN113933252B - Quality detection method of medicinal dendrobium nobile medicinal material - Google Patents
Quality detection method of medicinal dendrobium nobile medicinal material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 74
- 238000001514 detection method Methods 0.000 title claims abstract description 33
- 240000004638 Dendrobium nobile Species 0.000 title claims description 19
- 241001523681 Dendrobium Species 0.000 claims abstract description 121
- 239000000843 powder Substances 0.000 claims abstract description 52
- 238000000605 extraction Methods 0.000 claims abstract description 30
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims abstract 11
- 239000000523 sample Substances 0.000 claims description 103
- 239000000243 solution Substances 0.000 claims description 97
- 238000003756 stirring Methods 0.000 claims description 72
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 36
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 239000013068 control sample Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 25
- RYAHJFGVOCZDEI-UFFNCVEVSA-N Dendrobine Chemical compound C([C@H]1CC[C@@H]2[C@@]31C)N(C)[C@@H]3[C@H]1[C@@H](C(C)C)[C@@H]2C(=O)O1 RYAHJFGVOCZDEI-UFFNCVEVSA-N 0.000 claims description 23
- RYAHJFGVOCZDEI-CZKZLRAZSA-N dendrobine Natural products O=C1O[C@@H]2[C@H](C(C)C)[C@H]1[C@H]1[C@@]3(C)[C@@H]2N(C)C[C@H]3CC1 RYAHJFGVOCZDEI-CZKZLRAZSA-N 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000002137 ultrasound extraction Methods 0.000 claims description 21
- 239000011148 porous material Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- VADKRMSMGWJZCF-UHFFFAOYSA-N 2-bromophenol Chemical compound OC1=CC=CC=C1Br VADKRMSMGWJZCF-UHFFFAOYSA-N 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 12
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 238000002835 absorbance Methods 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 claims description 7
- 238000002798 spectrophotometry method Methods 0.000 claims description 7
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims 2
- 239000013074 reference sample Substances 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 abstract description 2
- 241000026010 Dendrobium candidum Species 0.000 description 12
- 239000012528 membrane Substances 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- UXDFUVFNIAJEGM-UHFFFAOYSA-N 2-methoxy-5-[2-(3,4,5-trimethoxyphenyl)ethyl]phenol Chemical compound C1=C(O)C(OC)=CC=C1CCC1=CC(OC)=C(OC)C(OC)=C1 UXDFUVFNIAJEGM-UHFFFAOYSA-N 0.000 description 2
- NQPYLTZHMORTPV-UHFFFAOYSA-M C1(=CC=CC=C1)O.[Br-].[K+] Chemical compound C1(=CC=CC=C1)O.[Br-].[K+] NQPYLTZHMORTPV-UHFFFAOYSA-M 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001471 micro-filtration Methods 0.000 description 2
- QWUWMCYKGHVNAV-UHFFFAOYSA-N 1,2-dihydrostilbene Chemical group C=1C=CC=CC=1CCC1=CC=CC=C1 QWUWMCYKGHVNAV-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N21/3151—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths using two sources of radiation of different wavelengths
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N2021/3155—Measuring in two spectral ranges, e.g. UV and visible
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- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Toxicology (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Extraction Or Liquid Replacement (AREA)
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Abstract
The invention belongs to the field of medicinal material detection, in particular to a quality detection method of medicinal dendrobium, which aims at the problems of low extraction rate and influence on detection effect of the existing method and provides the following scheme that the method comprises the following steps: obtaining a medicinal dendrobium medicinal material sample, crushing the medicinal dendrobium medicinal material sample to prepare dendrobium powder, filtering the dendrobium powder by using a 60-mesh sieve to obtain dendrobium powder passing through the 60-mesh sieve, weighing 5 g of the dendrobium powder, primarily extracting components in dendrobium by using a first solution, then secondarily concentrating and extracting the primary extract by using a second solution, and finally secondarily extracting by using a third solution, so that effective components in dendrobium can be fully extracted, the concentration and the extraction rate of a sample extract are improved, the detection effect is improved, and other types of dendrobium are adopted as comparative examples, so that different types of dendrobium can be compared, and multiple detection is avoided.
Description
Technical Field
The invention relates to the technical field of medicinal material detection, in particular to a quality detection method of medicinal dendrobium.
Background
Herba Dendrobii is perennial herb plant of Dendrobium of Orchidaceae, and its main medicinal part is fresh or dry stem, and is mainly distributed in Anhui, zhejiang, guangxi, hunan, yunnan, guizhou, etc. The patent with the application number of CN201410542575.6 discloses a quality detection method of dendrobium candidum, which is simple, easy to implement and good in repeatability, can accurately reflect the quality of the dendrobium candidum, further improves the quality standard of the dendrobium candidum, makes up for the defect that the quality evaluation of the dendrobium candidum lacks a detection method for fat-soluble characteristic components represented by bibenzyl, and ensures that the quality detection technology of the dendrobium candidum is more scientific and reasonable. The detection method can effectively control the quality of the dendrobium candidum medicinal material, thereby ensuring the safety, stability and effectiveness of clinical application of the dendrobium candidum medicinal material.
However, the quality detection method of the dendrobium candidum medicinal material also has some problems, for example, the extraction concentration of dendrobium candidum components is low, only a small part of components can be extracted, the quality of dendrobium candidum is difficult to accurately measure, the detection effect is affected, and the dendrobium candidum medicinal material quality detection method cannot be compared with other types of dendrobium candidum medicinal materials by using a solution prepared from erianin as a comparison example and needs multiple detection.
Disclosure of Invention
Based on the problems of low extraction concentration of dendrobium components, influence on detection effect and need of multiple detection in the background technology, the invention provides a quality detection method of medicinal dendrobium medicinal materials.
The invention provides a quality detection method of medicinal dendrobium, which comprises the following steps:
s1: obtaining a medicinal dendrobium medicinal material sample, crushing the medicinal dendrobium medicinal material sample to prepare dendrobium powder, filtering the dendrobium powder by using a 60-mesh sieve to obtain dendrobium powder passing through the 60-mesh sieve, and weighing 5 g of dendrobium powder;
s2: obtaining 200-250 ml of 50% ethanol, 150-160 ml of acetic acid, 100-110 ml of chloroform, 50-60 ml of diethyl ether and 50-60 ml of propanol, mixing the two to prepare a first solution, pouring the first solution into a stirring container, adding the weighed dendrobium powder into the stirring container, stirring until the dendrobium powder is completely dissolved into the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, and drying the extract after extraction to obtain a primary extract;
s3: adding a second solution into the primary extract, wherein the second solution consists of 150 ml-200 ml of 10% ammonia water, 15 g-25 g of sodium hydroxide and 5 g-15 g of potassium hydrogen phthalate, stirring uniformly, controlling the stirring time to be 10 minutes-15 minutes, performing rotary drying at 60-65 ℃, then adding 50ml of a third solution, stirring uniformly, wherein the third solution is a mixed solution of chloroform and methanol, sealing and standing for 30 minutes, and filtering the solution after standing to obtain a sample extract;
s4: obtaining a control sample containing dendrobine, pouring the control sample containing dendrobine into the prepared first solution, extracting by ultrasonic extraction equipment after stirring, adding the prepared second solution, uniformly stirring, drying, adding the third solution, uniformly stirring, standing and filtering to obtain a contrast extract;
s5: and (3) obtaining a sample extract and a comparison extract, respectively adding a bromophenol green solution into the sample extract and the comparison extract, uniformly stirring, and respectively measuring the absorbance of the sample extract and the comparison extract at the wavelength of 620nm by adopting an ultraviolet spectrophotometry to obtain the quality of the medicinal dendrobium.
Preferably, in the step S1, the obtained medicinal dendrobium sample needs to be screened in advance to remove unqualified materials, and then is cleaned and dried to be used as a sample.
Preferably, in the step S1, when the medicinal dendrobium sample is crushed, the medicinal dendrobium sample is first put into a blade crusher to be primarily crushed, and then the crushed medicinal dendrobium sample is poured into a grinding device to be ground.
Preferably, in the step S2, after the dendrobium powder is added, the stirring container is closed, and then stirring is carried out, wherein the stirring temperature is controlled to be 20-35 ℃, and the stirring time is controlled to be 5-10 minutes.
Preferably, in S2, the ultrasonic frequency is controlled between 28KHz and 30KHz, the power of the ultrasonic extraction equipment is controlled between 400W and 450W, and the extraction time is controlled between 45 minutes and 60 minutes.
Preferably, in the step S2, the extract is in a rotating state during drying, and the drying temperature is controlled to be 60-65 ℃.
Preferably, in S3, chloroform and methanol in the third solution are mixed according to a ratio of 9:1.
Preferably, in S3, the filtration is performed by using a microfiltration membrane, and the pore size of the microfiltration membrane is selected to be 0.50 μm.
Preferably, in S4, the control sample containing dendrobine may be other types of dendrobine, and the extraction step of the control sample is identical to the extraction step of the sample extract.
Preferably, in S5, the weights of the obtained sample extract and the comparative extract are required to be identical, the addition amount of the bromopotassium phenol green solution is 5ml, and 0.06% bromopotassium phenol green solution is selected.
The invention has the beneficial effects that:
the components in the dendrobe are initially extracted through the first solution, then the primary extract is subjected to concentration extraction again through the second solution, and finally the third solution is used for extracting again, so that the effective components in the dendrobe can be fully extracted, the concentration and the extraction rate of the sample extract are improved, the detection effect is improved, other types of dendrobe are adopted as comparison examples, different types of dendrobe can be compared, and multiple detection is avoided.
Drawings
Fig. 1 is a flow chart of the operation proposed by the present invention.
Detailed Description
The invention is further illustrated below in connection with specific embodiments.
Referring to fig. 1, embodiment one
The embodiment provides a quality detection method of medicinal dendrobium medicinal materials, which comprises the following steps of:
s1: obtaining a medicinal dendrobium medicinal material sample, wherein the obtained medicinal dendrobium medicinal material sample is required to be screened in advance to remove unqualified materials, then the medicinal dendrobium medicinal material sample is cleaned and dried to be used as a sample, the medicinal dendrobium medicinal material sample is crushed to obtain dendrobium powder, the dendrobium powder is filtered by a 60-mesh sieve to obtain the dendrobium powder passing through the 60-mesh sieve, 5 g of the dendrobium powder is weighed, when the medicinal dendrobium medicinal material sample is crushed, the medicinal dendrobium medicinal material sample is required to be put into a blade type crusher for preliminary crushing, and the crushed medicinal dendrobium medicinal material sample is poured into grinding equipment for grinding;
s2: obtaining 250ml of 50% ethanol, 160ml of acetic acid, 110ml of chloroform, 60ml of diethyl ether and 60ml of propanol, mixing the ethanol, the acetic acid, the chloroform, the 60ml of diethyl ether and the 60ml of propanol to prepare a first solution, pouring the first solution into a stirring container, adding the weighed dendrobium powder into the stirring container, stirring the dendrobium powder, sealing the stirring container, stirring the dendrobium powder, controlling the stirring temperature to be 20-35 ℃ and the stirring time to be 5-10 minutes until the dendrobium powder is completely dissolved into the mixed solution, pouring the mixed solution into an ultrasonic extraction device, controlling the ultrasonic frequency to be 28-30 KHz, controlling the power of the ultrasonic extraction device to be 400-450W, controlling the extraction time to be 45-60 minutes, drying the extract after the extraction, and controlling the drying temperature to be 60-65 ℃ to obtain a primary extract;
s3: adding a second solution into the primary extract, wherein the second solution consists of 180ml of 10% ammonia water, 25 g of sodium hydroxide and 15 g of potassium hydrogen phthalate, stirring uniformly, controlling the stirring time to be 10-15 minutes, performing rotary drying at 60-65 ℃, then adding 50ml of a third solution, stirring uniformly, mixing the third solution with chloroform and methanol according to the ratio of 9:1, sealing and standing for 30 minutes, filtering the solution after standing, and filtering by using a micro-pore filter membrane, wherein the pore diameter of the micro-pore filter membrane is 0.50 microns, thus obtaining a sample extract;
s4: obtaining a control sample containing dendrobine, wherein the control sample containing dendrobine can be selected from other types of dendrobines, the extraction step of the control sample is consistent with that of a sample extract, the control sample containing dendrobine is poured into a prepared first solution, stirred and extracted by ultrasonic extraction equipment, then a prepared second solution is added, uniformly stirred and dried, then a third solution is added, uniformly stirred, and the mixture is left to stand and filtered to obtain a comparison extract;
s5: obtaining a sample extract and a comparison extract, respectively adding a bromophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract and the weight of the comparison extract are required to be consistent, the adding amount of the bromophenol green solution is 5ml, and 0.06% bromophenol green solution is selected, after the sample extract and the comparison extract are uniformly stirred, the absorbance of the sample extract and the comparison extract at the wavelength of 620nm is respectively measured by adopting an ultraviolet spectrophotometry, so that the quality of medicinal dendrobium nobile can be obtained.
Referring to FIG. 1, embodiment II
The embodiment provides a quality detection method of medicinal dendrobium medicinal materials, which comprises the following steps of:
s1: obtaining a medicinal dendrobium medicinal material sample, wherein the obtained medicinal dendrobium medicinal material sample is required to be screened in advance to remove unqualified materials, then the medicinal dendrobium medicinal material sample is cleaned and dried to be used as a sample, the medicinal dendrobium medicinal material sample is crushed to obtain dendrobium powder, the dendrobium powder is filtered by a 60-mesh sieve to obtain the dendrobium powder passing through the 60-mesh sieve, 5 g of the dendrobium powder is weighed, when the medicinal dendrobium medicinal material sample is crushed, the medicinal dendrobium medicinal material sample is required to be put into a blade type crusher for preliminary crushing, and the crushed medicinal dendrobium medicinal material sample is poured into grinding equipment for grinding;
s2: obtaining 250ml of 50% ethanol, 160ml of acetic acid, 100ml of chloroform, 52ml of diethyl ether and 56ml of propanol, mixing the ethanol, the acetic acid, the chloroform and the 52ml of diethyl ether to prepare a first solution, pouring the first solution into a stirring container, adding the weighed dendrobium powder into the stirring container, stirring the dendrobium powder, sealing the stirring container, stirring the dendrobium powder, controlling the stirring temperature to be 20-35 ℃ and the stirring time to be 5-10 minutes until the dendrobium powder is completely dissolved into a mixed solution, pouring the mixed solution into an ultrasonic extraction device, controlling the ultrasonic frequency to be 28 KHz-30 KHz, controlling the power of the ultrasonic extraction device to be 400-450W, controlling the extraction time to be 45-60 minutes, drying the extract after the extraction, and controlling the extract to be in a rotating state when the extract is dried, and controlling the drying temperature to be 60-65 ℃ to obtain a primary extract;
s3: adding a second solution into the primary extract, wherein the second solution consists of 170ml of 10% ammonia water, 21 g of sodium hydroxide and 12 g of potassium hydrogen phthalate, stirring uniformly, controlling the stirring time to be 10-15 minutes, performing rotary drying at 60-65 ℃, then adding 50ml of a third solution, stirring uniformly, mixing the third solution with chloroform and methanol according to the ratio of 9:1, sealing and standing for 30 minutes, filtering the solution after standing, and filtering by using a micro-pore filter membrane, wherein the pore diameter of the micro-pore filter membrane is 0.50 micrometer, thus obtaining a sample extract;
s4: obtaining a control sample containing dendrobine, wherein the control sample containing dendrobine can be selected from other types of dendrobines, the extraction step of the control sample is consistent with that of a sample extract, the control sample containing dendrobine is poured into a prepared first solution, stirred and extracted by ultrasonic extraction equipment, then a prepared second solution is added, uniformly stirred and dried, then a third solution is added, uniformly stirred, and the mixture is left to stand and filtered to obtain a comparison extract;
s5: obtaining a sample extract and a comparison extract, respectively adding a bromophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract and the weight of the comparison extract are required to be consistent, the adding amount of the bromophenol green solution is 5ml, and 0.06% bromophenol green solution is selected, after the sample extract and the comparison extract are uniformly stirred, the absorbance of the sample extract and the comparison extract at the wavelength of 620nm is respectively measured by adopting an ultraviolet spectrophotometry, so that the quality of medicinal dendrobium nobile can be obtained.
Referring to fig. 1, embodiment three
The embodiment provides a quality detection method of medicinal dendrobium medicinal materials, which comprises the following steps of:
s1: obtaining a medicinal dendrobium medicinal material sample, wherein the obtained medicinal dendrobium medicinal material sample is required to be screened in advance to remove unqualified materials, then the medicinal dendrobium medicinal material sample is cleaned and dried to be used as a sample, the medicinal dendrobium medicinal material sample is crushed to obtain dendrobium powder, the dendrobium powder is filtered by a 60-mesh sieve to obtain the dendrobium powder passing through the 60-mesh sieve, 5 g of the dendrobium powder is weighed, when the medicinal dendrobium medicinal material sample is crushed, the medicinal dendrobium medicinal material sample is required to be put into a blade type crusher for preliminary crushing, and the crushed medicinal dendrobium medicinal material sample is poured into grinding equipment for grinding;
s2: obtaining 230ml of 50% ethanol, 156ml of acetic acid, 106ml of chloroform, 56ml of diethyl ether and 56ml of propanol, mixing the two to prepare a first solution, pouring the first solution into a stirring container, adding the weighed dendrobium powder into the stirring container, stirring the mixture, sealing the stirring container, stirring the mixture at a temperature of between 20 and 35 ℃ for 5 to 10 minutes until the dendrobium powder is completely dissolved into the mixed solution, pouring the mixed solution into an ultrasonic extraction device, controlling the ultrasonic frequency to between 28 and 30KHz, controlling the power of the ultrasonic extraction device to between 400 and 450W, controlling the extraction time to between 45 and 60 minutes, drying the extract after the extraction, and controlling the temperature of the extract to between 60 and 65 ℃ in a rotating state during the drying to obtain a primary extract;
s3: adding a second solution into the primary extract, wherein the second solution consists of 180ml of 10% ammonia water, 19 g of sodium hydroxide and 9 g of potassium hydrogen phthalate, stirring uniformly, controlling the stirring time to be 10-15 minutes, performing rotary drying at 60-65 ℃, then adding 50ml of a third solution, stirring uniformly, mixing the third solution with chloroform and methanol according to the ratio of 9:1, sealing and standing for 30 minutes, filtering the solution after standing, and filtering by using a micro-pore filter membrane, wherein the pore diameter of the micro-pore filter membrane is 0.50 micrometer, thus obtaining a sample extract;
s4: obtaining a control sample containing dendrobine, wherein the control sample containing dendrobine can be selected from other types of dendrobines, the extraction step of the control sample is consistent with that of a sample extract, the control sample containing dendrobine is poured into a prepared first solution, stirred and extracted by ultrasonic extraction equipment, then a prepared second solution is added, uniformly stirred and dried, then a third solution is added, uniformly stirred, and the mixture is left to stand and filtered to obtain a comparison extract;
s5: obtaining a sample extract and a comparison extract, respectively adding a bromophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract and the weight of the comparison extract are required to be consistent, the adding amount of the bromophenol green solution is 5ml, and 0.06% bromophenol green solution is selected, after the sample extract and the comparison extract are uniformly stirred, the absorbance of the sample extract and the comparison extract at the wavelength of 620nm is respectively measured by adopting an ultraviolet spectrophotometry, so that the quality of medicinal dendrobium nobile can be obtained.
Referring to fig. 1, embodiment four
The embodiment provides a quality detection method of medicinal dendrobium medicinal materials, which comprises the following steps of:
s1: obtaining a medicinal dendrobium medicinal material sample, wherein the obtained medicinal dendrobium medicinal material sample is required to be screened in advance to remove unqualified materials, then the medicinal dendrobium medicinal material sample is cleaned and dried to be used as a sample, the medicinal dendrobium medicinal material sample is crushed to obtain dendrobium powder, the dendrobium powder is filtered by a 60-mesh sieve to obtain the dendrobium powder passing through the 60-mesh sieve, 5 g of the dendrobium powder is weighed, when the medicinal dendrobium medicinal material sample is crushed, the medicinal dendrobium medicinal material sample is required to be put into a blade type crusher for preliminary crushing, and the crushed medicinal dendrobium medicinal material sample is poured into grinding equipment for grinding;
s2: obtaining 220ml of 50% ethanol, 152ml of acetic acid, 102ml of chloroform, 52ml of diethyl ether and 52ml of propanol, mixing the two to prepare a first solution, pouring the first solution into a stirring container, adding the weighed dendrobium powder into the stirring container, stirring the mixture, sealing the stirring container, stirring the mixture at a temperature of between 20 and 35 ℃ for 5 to 10 minutes until the dendrobium powder is completely dissolved into the mixed solution, pouring the mixed solution into an ultrasonic extraction device, controlling the ultrasonic frequency to between 28 and 30KHz, controlling the power of the ultrasonic extraction device to between 400 and 450W, controlling the extraction time to between 45 and 60 minutes, drying the extract after the extraction, and controlling the temperature of the extract to between 60 and 65 ℃ in a rotating state during the drying to obtain a primary extract;
s3: adding a second solution into the primary extract, wherein the second solution consists of 190ml of 10% ammonia water, 17 g of sodium hydroxide and 7 g of potassium hydrogen phthalate, stirring uniformly, controlling the stirring time to be 10-15 minutes, performing rotary drying at 60-65 ℃, then adding 50ml of a third solution, stirring uniformly, mixing the third solution with chloroform and methanol according to the ratio of 9:1, sealing and standing for 30 minutes, filtering the solution after standing, and filtering by using a micro-pore filter membrane, wherein the pore diameter of the micro-pore filter membrane is 0.50 micrometer, thus obtaining a sample extract;
s4: obtaining a control sample containing dendrobine, wherein the control sample containing dendrobine can be selected from other types of dendrobines, the extraction step of the control sample is consistent with that of a sample extract, the control sample containing dendrobine is poured into a prepared first solution, stirred and extracted by ultrasonic extraction equipment, then a prepared second solution is added, uniformly stirred and dried, then a third solution is added, uniformly stirred, and the mixture is left to stand and filtered to obtain a comparison extract;
s5: obtaining a sample extract and a comparison extract, respectively adding a bromophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract and the weight of the comparison extract are required to be consistent, the adding amount of the bromophenol green solution is 5ml, and 0.06% bromophenol green solution is selected, after the sample extract and the comparison extract are uniformly stirred, the absorbance of the sample extract and the comparison extract at the wavelength of 620nm is respectively measured by adopting an ultraviolet spectrophotometry, so that the quality of medicinal dendrobium nobile can be obtained.
Referring to fig. 1, embodiment five
The embodiment provides a quality detection method of medicinal dendrobium medicinal materials, which comprises the following steps of:
s1: obtaining a medicinal dendrobium medicinal material sample, wherein the obtained medicinal dendrobium medicinal material sample is required to be screened in advance to remove unqualified materials, then the medicinal dendrobium medicinal material sample is cleaned and dried to be used as a sample, the medicinal dendrobium medicinal material sample is crushed to obtain dendrobium powder, the dendrobium powder is filtered by a 60-mesh sieve to obtain the dendrobium powder passing through the 60-mesh sieve, 5 g of the dendrobium powder is weighed, when the medicinal dendrobium medicinal material sample is crushed, the medicinal dendrobium medicinal material sample is required to be put into a blade type crusher for preliminary crushing, and the crushed medicinal dendrobium medicinal material sample is poured into grinding equipment for grinding;
s2: obtaining 200ml of 50% ethanol, 150ml of acetic acid, 100ml of chloroform, 50ml of diethyl ether and 50ml of propanol, mixing the two to prepare a first solution, pouring the first solution into a stirring container, adding the weighed dendrobium powder into the stirring container, stirring the mixture, sealing the stirring container, stirring the mixture at a temperature of between 20 and 35 ℃ for 5 to 10 minutes until the dendrobium powder is completely dissolved into the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, controlling the ultrasonic frequency to between 28 and 30KHz, controlling the power of the ultrasonic extraction equipment to between 400 and 450W, controlling the extraction time to between 45 and 60 minutes, drying the extract after the extraction, and controlling the temperature of the extract to between 60 and 65 ℃ in a rotating state during the drying to obtain a primary extract;
s3: adding a second solution into the primary extract, wherein the second solution consists of 200ml of 10% ammonia water, 15 g of sodium hydroxide and 5 g of potassium hydrogen phthalate, stirring uniformly, controlling the stirring time to be 10-15 minutes, performing rotary drying at 60-65 ℃, then adding 50ml of a third solution, stirring uniformly, mixing the third solution with chloroform and methanol according to the ratio of 9:1, sealing and standing for 30 minutes, filtering the solution after standing, and filtering by using a micro-pore filter membrane, wherein the pore diameter of the micro-pore filter membrane is 0.50 microns, thus obtaining a sample extract;
s4: obtaining a control sample containing dendrobine, wherein the control sample containing dendrobine can be selected from other types of dendrobines, the extraction step of the control sample is consistent with that of a sample extract, the control sample containing dendrobine is poured into a prepared first solution, stirred and extracted by ultrasonic extraction equipment, then a prepared second solution is added, uniformly stirred and dried, then a third solution is added, uniformly stirred, and the mixture is left to stand and filtered to obtain a comparison extract;
s5: obtaining a sample extract and a comparison extract, respectively adding a bromophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract and the weight of the comparison extract are required to be consistent, the adding amount of the bromophenol green solution is 5ml, and 0.06% bromophenol green solution is selected, after the sample extract and the comparison extract are uniformly stirred, the absorbance of the sample extract and the comparison extract at the wavelength of 620nm is respectively measured by adopting an ultraviolet spectrophotometry, so that the quality of medicinal dendrobium nobile can be obtained.
Comparing the conventional quality detection method of the medicinal dendrobium medicinal materials with the quality detection methods of the medicinal dendrobium medicinal materials in the first to fifth embodiments, the quality detection methods of the medicinal dendrobium medicinal materials in the first to fifth embodiments are shown in the following table:
the above table shows that the extraction rate of the quality detection method of the medicinal dendrobium medicinal material is obviously improved, and the second best embodiment is implemented.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The quality detection method of the medicinal dendrobium nobile medicinal material is characterized by comprising the following steps of:
s1: obtaining a medicinal dendrobium medicinal material sample, crushing the medicinal dendrobium medicinal material sample to prepare dendrobium powder, filtering the dendrobium powder by using a 60-mesh sieve to obtain dendrobium powder passing through the 60-mesh sieve, and weighing 5 g of dendrobium powder;
s2: obtaining 200-250 ml of 50% ethanol, 150-160 ml of acetic acid, 100-110 ml of chloroform, 50-60 ml of diethyl ether and 50-60 ml of propanol, mixing the two to prepare a first solution, pouring the first solution into a stirring container, adding the weighed dendrobium powder into the stirring container, stirring until the dendrobium powder is completely dissolved into the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, and drying the extract after extraction to obtain a primary extract;
s3: adding a second solution into the primary extract, wherein the second solution consists of 150 ml-200 ml of 10% ammonia water, 15 g-25 g of sodium hydroxide and 5 g-15 g of potassium hydrogen phthalate, stirring uniformly, controlling the stirring time to be 10 minutes-15 minutes, performing rotary drying at 60-65 ℃, then adding 50ml of a third solution, stirring uniformly, wherein the third solution is a mixed solution of chloroform and methanol, sealing and standing for 30 minutes, and filtering the solution after standing to obtain a sample extract;
s4: obtaining a control sample containing dendrobine, pouring the control sample containing dendrobine into the prepared first solution, extracting by ultrasonic extraction equipment after stirring, adding the prepared second solution, uniformly stirring, drying, adding the third solution, uniformly stirring, standing and filtering to obtain a contrast extract;
s5: and (3) obtaining a sample extract and a comparison extract, respectively adding a bromophenol green solution into the sample extract and the comparison extract, uniformly stirring, and respectively measuring the absorbance of the sample extract and the comparison extract at the wavelength of 620nm by adopting an ultraviolet spectrophotometry to obtain the quality of the medicinal dendrobium.
2. The method for detecting the quality of medicinal dendrobium according to claim 1, wherein in S1, the obtained medicinal dendrobium sample is required to be screened in advance, unqualified materials are removed, and then the obtained medicinal dendrobium sample is cleaned and dried to obtain the medicinal dendrobium sample.
3. The method for detecting the quality of a dendrobium nobile medicinal material according to claim 1, wherein in S1, when the dendrobium nobile medicinal material sample is crushed, the dendrobium nobile medicinal material sample is first put into a blade crusher to be primarily crushed, and then the crushed dendrobium nobile medicinal material sample is poured into a grinding device to be ground.
4. The method for detecting the quality of medicinal dendrobium nobile according to claim 1, wherein in the step S2, after adding dendrobium nobile powder, a stirring container is closed, and then stirring is performed, wherein the stirring temperature is controlled to be 20-35 ℃, and the stirring time is controlled to be 5-10 minutes.
5. The method for detecting the quality of dendrobium nobile according to claim 1, wherein in the step S2, the ultrasonic frequency is controlled between 28KHz and 30KHz, the power of the ultrasonic extraction device is controlled between 400W and 450W, and the extraction time is controlled between 45 minutes and 60 minutes.
6. The method for detecting the quality of dendrobium nobile medicinal material according to claim 1, wherein in the step S2, the extract is in a rotating state during drying, and the drying temperature is controlled to be 60-65 ℃.
7. The method for detecting the quality of dendrobium nobile as claimed in claim 1, wherein in the step S3, chloroform and methanol in the third solution are mixed according to a ratio of 9:1.
8. The method for detecting the quality of dendrobium nobile as claimed in claim 1, wherein in the step S3, a micro-pore filter is adopted for filtering, and the pore diameter of the micro-pore filter is 0.50 micron.
9. The method according to claim 1, wherein in S4, the reference sample containing dendrobine may be other types of dendrobine, and the extraction step of the reference sample is identical to the extraction step of the sample extract.
10. The method for detecting the quality of dendrobium nobile medicinal material according to claim 1, wherein in the step S5, the weight of the obtained sample extract and the weight of the obtained reference extract are required to be consistent, the adding amount of the bromopotassium green solution is 5ml, and 0.06% of the bromopotassium green solution is selected.
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| CN104237151A (en) * | 2014-10-14 | 2014-12-24 | 宁波枫康生物科技有限公司 | Mass detection method for dendrobium officinale medicine |
| CN105424850A (en) * | 2015-11-05 | 2016-03-23 | 北京蓝标一成科技有限公司 | Quality evaluation method for dendrobe medicinal material |
| CN110361346A (en) * | 2019-07-19 | 2019-10-22 | 浙江大学 | A kind of quality determining method of dendrobium candidum medicinal material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104237151A (en) * | 2014-10-14 | 2014-12-24 | 宁波枫康生物科技有限公司 | Mass detection method for dendrobium officinale medicine |
| CN105424850A (en) * | 2015-11-05 | 2016-03-23 | 北京蓝标一成科技有限公司 | Quality evaluation method for dendrobe medicinal material |
| CN110361346A (en) * | 2019-07-19 | 2019-10-22 | 浙江大学 | A kind of quality determining method of dendrobium candidum medicinal material |
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