CN113933252A - Quality detection method for medicinal dendrobium medicinal material - Google Patents
Quality detection method for medicinal dendrobium medicinal material Download PDFInfo
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- CN113933252A CN113933252A CN202111192431.9A CN202111192431A CN113933252A CN 113933252 A CN113933252 A CN 113933252A CN 202111192431 A CN202111192431 A CN 202111192431A CN 113933252 A CN113933252 A CN 113933252A
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- 239000000463 material Substances 0.000 title claims abstract description 85
- 241001523681 Dendrobium Species 0.000 title claims abstract description 47
- 238000001514 detection method Methods 0.000 title claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 52
- 238000000605 extraction Methods 0.000 claims abstract description 30
- 230000000052 comparative effect Effects 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract 10
- 239000000243 solution Substances 0.000 claims description 126
- 239000000523 sample Substances 0.000 claims description 100
- 238000003756 stirring Methods 0.000 claims description 76
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 42
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 30
- 239000013068 control sample Substances 0.000 claims description 28
- 238000001914 filtration Methods 0.000 claims description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 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 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229960001701 chloroform Drugs 0.000 claims description 21
- 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 21
- 239000011259 mixed solution Substances 0.000 claims description 21
- 238000002137 ultrasound extraction Methods 0.000 claims description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 19
- WKENNNAGELEZFD-UHFFFAOYSA-N OC(C=CC=C1Br)=C1[K] Chemical compound OC(C=CC=C1Br)=C1[K] WKENNNAGELEZFD-UHFFFAOYSA-N 0.000 claims description 19
- 240000004638 Dendrobium nobile Species 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 14
- 238000001471 micro-filtration Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- 241001076416 Dendrobium tosaense Species 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 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
- 239000011148 porous material Substances 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
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 7
- 238000002798 spectrophotometry method Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 239000004480 active ingredient Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 4
- 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
- QWUWMCYKGHVNAV-UHFFFAOYSA-N 1,2-dihydrostilbene Chemical group C=1C=CC=CC=1CCC1=CC=CC=C1 QWUWMCYKGHVNAV-UHFFFAOYSA-N 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
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
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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
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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
- G01N2021/3155—Measuring in two spectral ranges, e.g. UV and visible
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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, aiming at the problems of low extraction rate and influence on detection effect of the existing method, the following scheme is proposed, which comprises the following steps: obtain medicinal dendrobe medicinal material sample, smash medicinal dendrobe medicinal material sample and make the dendrobe powder, then utilize 60 mesh sieve to filter the dendrobe powder, obtain the dendrobe powder that passes through 60 mesh sieve, 5 grams are got from the centre, the composition in the dendrobe is tentatively extracted through first solution, then carry out the concentrated extraction once more to preliminary extract through the second solution, use the third solution to extract once more at last, make the active ingredient in the dendrobe can fully draw out, promote the concentration and the extraction rate of sample extract, increase the effect that detects, and adopt other kinds of dendrobe as the comparative example, can contrast different kinds of dendrobe, avoid many times to detect.
Description
Technical Field
The invention relates to the technical field of medicinal material detection, in particular to a quality detection method of a medicinal dendrobe medicinal material.
Background
Herba Dendrobii is perennial herb of Dendrobium of Orchidaceae, and its main medicinal parts are fresh or dry stems, and are mainly distributed in Anhui, Zhejiang, Guangxi, Hunan, Yunnan, Guizhou, etc. The patent with the application number of CN201410542575.6 discloses a quality detection method for a dendrobium officinale medicinal material, which is simple, convenient and easy to implement, has good repeatability, can exactly reflect the quality of the dendrobium officinale medicinal material, further improves the quality standard of the dendrobium officinale medicinal material, makes up the defect that a detection method for fat-soluble characteristic components represented by bibenzyl is lacked in the quality evaluation of the dendrobium officinale, and enables the quality detection technology of the dendrobium officinale medicinal material to be more scientific and reasonable. The detection method can effectively control the quality of the dendrobium officinale medicinal material, thereby ensuring the safety, stability and effectiveness of clinical application of the dendrobium officinale medicinal material.
However, the quality detection method for the dendrobium officinale medicinal material also has some problems, for example, the extraction concentration of the dendrobium officinale ingredient is low, only a small part of the ingredient can be extracted, the quality of the dendrobium officinale is difficult to accurately measure, the detection effect is influenced, and the solution prepared by using erianin as a comparative example cannot be compared with other types of dendrobium officinale medicinal materials, so that multiple detections are needed.
Disclosure of Invention
Based on the problems of low extraction concentration of dendrobium components, influence on detection effect and need of repeated 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, then 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 the 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 ether and 50-60 ml of propanol, mixing to prepare a first solution, pouring the first solution into a stirring container, adding the weighed dendrobe powder into the first solution, stirring until the dendrobe powder is completely dissolved in the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, and drying the extract after extraction to obtain a primary extracting solution;
s3: adding a second solution into the primary extracting solution, wherein the second solution consists of 150-200 ml of 10% ammonia water, 15-25 g of sodium hydroxide and 5-15 g of potassium hydrogen phthalate, uniformly stirring, controlling the stirring time to be 10-15 minutes, carrying out rotary drying at the temperature of 60-65 ℃, then adding 50ml of a third solution, uniformly stirring, wherein the third solution is a mixed solution of trichloromethane and methanol, hermetically standing for 30 minutes, and filtering the solution after standing to obtain a sample extract;
s4: obtaining a dendrobine-containing control sample, pouring the dendrobine-containing control sample into the prepared first solution, stirring, extracting by using ultrasonic extraction equipment, adding the prepared second solution, uniformly stirring, drying, adding the third solution, uniformly stirring, standing and filtering to obtain a comparative extracting solution;
s5: and (3) obtaining a sample extract and a comparison extract, respectively adding a bromokaliophenol 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, so that the quality of the medicinal dendrobium nobile material can be obtained.
Preferably, in S1, the obtained sample of the medicinal dendrobium nobile material needs to be screened in advance to remove unqualified materials, and then cleaned and dried to obtain the sample.
Preferably, in S1, when the sample of the medicinal dendrobium nobile material is pulverized, it is required to put it into a blade type pulverizer for primary pulverization, and then pour the pulverized medicinal dendrobium nobile material sample into a grinding device for grinding.
Preferably, after the dendrobium powder is added in the S2, the stirring container is sealed, 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 to be 28KHz to 30KHz, the power of the ultrasonic extraction device is controlled to be 400W to 450W, and the extraction time is controlled to be 45 minutes to 60 minutes.
Preferably, in S2, the extract is in a rotating state during drying, and the drying temperature is controlled to be 60-65 ℃.
Preferably, in S3, the chloroform and the methanol in the third solution are mixed according to the 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 dendrobine-containing control sample can be selected from other types of dendrobines, and the extraction step of the control sample is identical to the extraction step of the sample extract.
Preferably, in S5, the weight of the sample extract and the weight of the comparative extract are required to be consistent, the addition amount of the green bromopotassium phenol solution is 5ml, and 0.06% green bromopotassium phenol solution is used.
The invention has the beneficial effects that:
the ingredients in the dendrobium nobile are preliminarily extracted through the first solution, then the preliminary extract is concentrated and extracted again through the second solution, and finally the third solution is used for re-extraction, so that the effective ingredients in the dendrobium nobile can be fully extracted, the concentration and the extraction rate of the sample extract are improved, the detection effect is increased, and the dendrobium nobile of other types is adopted as a comparative example, so that the dendrobium nobile of different types can be compared, and the repeated detection is avoided.
Drawings
Fig. 1 is a flow chart of the present invention.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Referring to FIG. 1, the first embodiment
The embodiment provides a quality detection method of medicinal dendrobium, which comprises the following steps:
s1: obtaining a medicinal dendrobe medicinal material sample, screening the obtained medicinal dendrobe medicinal material sample in advance, removing unqualified materials in the medicinal dendrobe medicinal material sample, cleaning and drying the medicinal dendrobe medicinal material sample to obtain a sample, crushing the medicinal dendrobe medicinal material sample to prepare dendrobe powder, filtering the dendrobe powder by using a 60-mesh sieve to obtain dendrobe powder passing through the 60-mesh sieve, weighing 5 g of the dendrobe powder, crushing the medicinal dendrobe medicinal material sample by putting the crushed medicinal dendrobe medicinal material sample into a blade type crusher for primary crushing, and pouring the crushed medicinal dendrobe medicinal material sample into grinding equipment for grinding;
s2: taking 250ml of 50% ethanol, 160ml of acetic acid, 110ml of chloroform, 60ml of diethyl ether and 60ml of propanol, mixing them to prepare a first solution, pouring the first solution into a stirring container, then adding the weighed dendrobium powder into the mixture for stirring, sealing the stirring container after adding the dendrobium powder, then stirring, controlling the stirring temperature at 20-35 ℃, controlling the stirring time at 5-10 minutes until the dendrobium powder is completely dissolved in the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, controlling the ultrasonic frequency to be 28 KHz-30 KHz, controlling the power of the ultrasonic extraction equipment to be 400W-450W, controlling the extraction time to be 45 minutes-60 minutes, drying the extract after extraction, controlling the drying temperature to be 60-65 ℃ and obtaining a primary extract;
s3: adding a second solution into the primary extracting solution, wherein the second solution consists of 180ml of 10% ammonia water, 25 g of sodium hydroxide and 15 g of potassium hydrogen phthalate, uniformly stirring, controlling the stirring time to be 10-15 minutes, carrying out rotary drying at the temperature of 60-65 ℃, then adding 50ml of a third solution, uniformly stirring, wherein the third solution is a mixed solution of trichloromethane and methanol, mixing the trichloromethane and the methanol in the third solution according to the ratio of 9:1, carrying out closed standing for 30 minutes, filtering the solution after standing, filtering by using a microfiltration membrane, and selecting the pore size of the microfiltration membrane to be 0.50 micron to obtain a sample extract;
s4: obtaining a dendrobine-containing control sample, wherein the dendrobine-containing control sample can be selected from other types of dendrobe, the extraction step of the control sample is consistent with that of the sample extract, the dendrobine-containing control sample is poured into the prepared first solution, the first solution is stirred and then extracted by ultrasonic extraction equipment, the prepared second solution is added, the second solution is stirred uniformly and then dried, the third solution is added and stirred uniformly, and the contrast extract is obtained after standing and filtering;
s5: and (3) obtaining a sample extract and a comparison extract, respectively adding a bromokaliophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract is consistent with that of the comparison extract, the addition amount of the bromokaliophenol green solution is 5ml, and 0.06% bromokaliophenol green solution is selected, and after uniformly stirring, respectively measuring the absorbance of the sample extract and the comparison extract at the wavelength of 620nm by adopting an ultraviolet spectrophotometry, so that the quality of the medicinal dendrobium medicinal material can be obtained.
Referring to FIG. 1, example II
The embodiment provides a quality detection method of medicinal dendrobium, which comprises the following steps:
s1: obtaining a medicinal dendrobe medicinal material sample, screening the obtained medicinal dendrobe medicinal material sample in advance, removing unqualified materials in the medicinal dendrobe medicinal material sample, cleaning and drying the medicinal dendrobe medicinal material sample to obtain a sample, crushing the medicinal dendrobe medicinal material sample to prepare dendrobe powder, filtering the dendrobe powder by using a 60-mesh sieve to obtain dendrobe powder passing through the 60-mesh sieve, weighing 5 g of the dendrobe powder, crushing the medicinal dendrobe medicinal material sample by putting the crushed medicinal dendrobe medicinal material sample into a blade type crusher for primary crushing, and pouring the crushed medicinal dendrobe medicinal material sample into grinding equipment for grinding;
s2: taking 250ml of 50% ethanol, 160ml of acetic acid, 100ml of chloroform, 52ml of diethyl ether and 56ml of propanol, mixing them to prepare a first solution, pouring the first solution into a stirring container, then adding the weighed dendrobium powder into the mixture for stirring, sealing the stirring container after adding the dendrobium powder, then stirring, controlling the stirring temperature at 20-35 ℃, controlling the stirring time at 5-10 minutes until the dendrobium powder is completely dissolved in the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, controlling the ultrasonic frequency to be 28 KHz-30 KHz, controlling the power of the ultrasonic extraction equipment to be 400W-450W, controlling the extraction time to be 45 minutes-60 minutes, drying the extract after extraction, controlling the drying temperature to be 60-65 ℃ and obtaining a primary extract;
s3: adding a second solution into the primary extracting solution, wherein the second solution consists of 170ml of 10% ammonia water, 21 g of sodium hydroxide and 12 g of potassium hydrogen phthalate, uniformly stirring, controlling the stirring time to be 10-15 minutes, carrying out rotary drying at the temperature of 60-65 ℃, then adding 50ml of a third solution, uniformly stirring, wherein the third solution is a mixed solution of trichloromethane and methanol, mixing the trichloromethane and the methanol in the third solution according to the ratio of 9:1, carrying out closed standing for 30 minutes, filtering the solution after standing, filtering by using a microfiltration membrane, and selecting the pore size of the microfiltration membrane to be 0.50 microns to obtain a sample extract;
s4: obtaining a dendrobine-containing control sample, wherein the dendrobine-containing control sample can be selected from other types of dendrobe, the extraction step of the control sample is consistent with that of the sample extract, the dendrobine-containing control sample is poured into the prepared first solution, the first solution is stirred and then extracted by ultrasonic extraction equipment, the prepared second solution is added, the second solution is stirred uniformly and then dried, the third solution is added and stirred uniformly, and the contrast extract is obtained after standing and filtering;
s5: and (3) obtaining a sample extract and a comparison extract, respectively adding a bromokaliophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract is consistent with that of the comparison extract, the addition amount of the bromokaliophenol green solution is 5ml, and 0.06% bromokaliophenol green solution is selected, and after uniformly stirring, respectively measuring the absorbance of the sample extract and the comparison extract at the wavelength of 620nm by adopting an ultraviolet spectrophotometry, so that the quality of the medicinal dendrobium medicinal material can be obtained.
Referring to FIG. 1, example III
The embodiment provides a quality detection method of medicinal dendrobium, which comprises the following steps:
s1: obtaining a medicinal dendrobe medicinal material sample, screening the obtained medicinal dendrobe medicinal material sample in advance, removing unqualified materials in the medicinal dendrobe medicinal material sample, cleaning and drying the medicinal dendrobe medicinal material sample to obtain a sample, crushing the medicinal dendrobe medicinal material sample to prepare dendrobe powder, filtering the dendrobe powder by using a 60-mesh sieve to obtain dendrobe powder passing through the 60-mesh sieve, weighing 5 g of the dendrobe powder, crushing the medicinal dendrobe medicinal material sample by putting the crushed medicinal dendrobe medicinal material sample into a blade type crusher for primary crushing, and pouring the crushed medicinal dendrobe medicinal material sample into grinding equipment for grinding;
s2: 230ml of 50% ethanol, 156ml of acetic acid, 106ml of chloroform, 56ml of diethyl ether and 56ml of propanol were taken, mixed to prepare a first solution, the first solution was poured into a stirring vessel, then adding the weighed dendrobium powder into the mixture for stirring, sealing the stirring container after adding the dendrobium powder, then stirring, controlling the stirring temperature at 20-35 ℃, controlling the stirring time at 5-10 minutes until the dendrobium powder is completely dissolved in the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, controlling the ultrasonic frequency to be 28 KHz-30 KHz, controlling the power of the ultrasonic extraction equipment to be 400W-450W, controlling the extraction time to be 45 minutes-60 minutes, drying the extract after extraction, controlling the drying temperature to be 60-65 ℃ and obtaining a primary extract;
s3: adding a second solution into the primary extracting solution, wherein the second solution consists of 180ml of 10% ammonia water, 19 g of sodium hydroxide and 9 g of potassium hydrogen phthalate, uniformly stirring, controlling the stirring time to be 10-15 minutes, carrying out rotary drying at the temperature of 60-65 ℃, then adding 50ml of a third solution, uniformly stirring, wherein the third solution is a mixed solution of trichloromethane and methanol, mixing the trichloromethane and the methanol in the third solution according to the ratio of 9:1, carrying out closed standing for 30 minutes, filtering the solution after standing, filtering by using a microfiltration membrane, and selecting the pore size of the microfiltration membrane to be 0.50 micron to obtain a sample extract;
s4: obtaining a dendrobine-containing control sample, wherein the dendrobine-containing control sample can be selected from other types of dendrobe, the extraction step of the control sample is consistent with that of the sample extract, the dendrobine-containing control sample is poured into the prepared first solution, the first solution is stirred and then extracted by ultrasonic extraction equipment, the prepared second solution is added, the second solution is stirred uniformly and then dried, the third solution is added and stirred uniformly, and the contrast extract is obtained after standing and filtering;
s5: and (3) obtaining a sample extract and a comparison extract, respectively adding a bromokaliophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract is consistent with that of the comparison extract, the addition amount of the bromokaliophenol green solution is 5ml, and 0.06% bromokaliophenol green solution is selected, and after uniformly stirring, respectively measuring the absorbance of the sample extract and the comparison extract at the wavelength of 620nm by adopting an ultraviolet spectrophotometry, so that the quality of the medicinal dendrobium medicinal material can be obtained.
Referring to FIG. 1, example No. four
The embodiment provides a quality detection method of medicinal dendrobium medicinal materials, which comprises the following steps:
s1: obtaining a medicinal dendrobe medicinal material sample, screening the obtained medicinal dendrobe medicinal material sample in advance, removing unqualified materials in the medicinal dendrobe medicinal material sample, cleaning and drying the medicinal dendrobe medicinal material sample to obtain a sample, crushing the medicinal dendrobe medicinal material sample to prepare dendrobe powder, filtering the dendrobe powder by using a 60-mesh sieve to obtain dendrobe powder passing through the 60-mesh sieve, weighing 5 g of the dendrobe powder, crushing the medicinal dendrobe medicinal material sample by putting the crushed medicinal dendrobe medicinal material sample into a blade type crusher for primary crushing, and pouring the crushed medicinal dendrobe medicinal material sample into grinding equipment for grinding;
s2: taking 220ml of 50% ethanol, 152ml of acetic acid, 102ml of chloroform, 52ml of diethyl ether and 52ml of propanol, mixing them to prepare a first solution, pouring the first solution into a stirring container, then adding the weighed dendrobium powder into the mixture for stirring, sealing the stirring container after adding the dendrobium powder, then stirring, controlling the stirring temperature at 20-35 ℃, controlling the stirring time at 5-10 minutes until the dendrobium powder is completely dissolved in the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, controlling the ultrasonic frequency to be 28 KHz-30 KHz, controlling the power of the ultrasonic extraction equipment to be 400W-450W, controlling the extraction time to be 45 minutes-60 minutes, drying the extract after extraction, controlling the drying temperature to be 60-65 ℃ and obtaining a primary extract;
s3: adding a second solution into the primary extracting solution, wherein the second solution consists of 190ml of 10% ammonia water, 17 g of sodium hydroxide and 7 g of potassium hydrogen phthalate, uniformly stirring, controlling the stirring time to be 10-15 minutes, carrying out rotary drying at the temperature of 60-65 ℃, then adding 50ml of a third solution, uniformly stirring, wherein the third solution is a mixed solution of trichloromethane and methanol, mixing the trichloromethane and the methanol in the third solution according to the ratio of 9:1, carrying out closed standing for 30 minutes, filtering the solution after standing, filtering by using a microfiltration membrane, and selecting the pore size of the microfiltration membrane to be 0.50 microns to obtain a sample extract;
s4: obtaining a dendrobine-containing control sample, wherein the dendrobine-containing control sample can be selected from other types of dendrobe, the extraction step of the control sample is consistent with that of the sample extract, the dendrobine-containing control sample is poured into the prepared first solution, the first solution is stirred and then extracted by ultrasonic extraction equipment, the prepared second solution is added, the second solution is stirred uniformly and then dried, the third solution is added and stirred uniformly, and the contrast extract is obtained after standing and filtering;
s5: and (3) obtaining a sample extract and a comparison extract, respectively adding a bromokaliophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract is consistent with that of the comparison extract, the addition amount of the bromokaliophenol green solution is 5ml, and 0.06% bromokaliophenol green solution is selected, and after uniformly stirring, respectively measuring the absorbance of the sample extract and the comparison extract at the wavelength of 620nm by adopting an ultraviolet spectrophotometry, so that the quality of the medicinal dendrobium medicinal material can be obtained.
Referring to FIG. 1, example V
The embodiment provides a quality detection method of medicinal dendrobium, which comprises the following steps:
s1: obtaining a medicinal dendrobe medicinal material sample, screening the obtained medicinal dendrobe medicinal material sample in advance, removing unqualified materials in the medicinal dendrobe medicinal material sample, cleaning and drying the medicinal dendrobe medicinal material sample to obtain a sample, crushing the medicinal dendrobe medicinal material sample to prepare dendrobe powder, filtering the dendrobe powder by using a 60-mesh sieve to obtain dendrobe powder passing through the 60-mesh sieve, weighing 5 g of the dendrobe powder, crushing the medicinal dendrobe medicinal material sample by putting the crushed medicinal dendrobe medicinal material sample into a blade type crusher for primary crushing, and pouring the crushed medicinal dendrobe medicinal material sample into grinding equipment for grinding;
s2: taking 200ml of 50% ethanol, 150ml of acetic acid, 100ml of chloroform, 50ml of diethyl ether and 50ml of propanol, mixing them to prepare a first solution, pouring the first solution into a stirring container, then adding the weighed dendrobium powder into the mixture for stirring, sealing the stirring container after adding the dendrobium powder, then stirring, controlling the stirring temperature at 20-35 ℃, controlling the stirring time at 5-10 minutes until the dendrobium powder is completely dissolved in the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, controlling the ultrasonic frequency to be 28 KHz-30 KHz, controlling the power of the ultrasonic extraction equipment to be 400W-450W, controlling the extraction time to be 45 minutes-60 minutes, drying the extract after extraction, controlling the drying temperature to be 60-65 ℃ and obtaining a primary extract;
s3: adding a second solution into the primary extracting solution, wherein the second solution consists of 200ml of 10% ammonia water, 15 g of sodium hydroxide and 5 g of potassium hydrogen phthalate, uniformly stirring, controlling the stirring time to be 10-15 minutes, carrying out rotary drying at the temperature of 60-65 ℃, then adding 50ml of a third solution, uniformly stirring, wherein the third solution is a mixed solution of trichloromethane and methanol, mixing the trichloromethane and the methanol in the third solution according to the ratio of 9:1, carrying out closed standing for 30 minutes, filtering the solution after standing, filtering by using a microfiltration membrane, and selecting the pore size of the microfiltration membrane to be 0.50 micrometer to obtain a sample extract;
s4: obtaining a dendrobine-containing control sample, wherein the dendrobine-containing control sample can be selected from other types of dendrobe, the extraction step of the control sample is consistent with that of the sample extract, the dendrobine-containing control sample is poured into the prepared first solution, the first solution is stirred and then extracted by ultrasonic extraction equipment, the prepared second solution is added, the second solution is stirred uniformly and then dried, the third solution is added and stirred uniformly, and the contrast extract is obtained after standing and filtering;
s5: and (3) obtaining a sample extract and a comparison extract, respectively adding a bromokaliophenol green solution into the sample extract and the comparison extract, wherein the weight of the obtained sample extract is consistent with that of the comparison extract, the addition amount of the bromokaliophenol green solution is 5ml, and 0.06% bromokaliophenol green solution is selected, and after uniformly stirring, respectively measuring the absorbance of the sample extract and the comparison extract at the wavelength of 620nm by adopting an ultraviolet spectrophotometry, so that the quality of the medicinal dendrobium medicinal material can be obtained.
Comparing the conventional quality detection method for medicinal dendrobe and the quality detection methods for medicinal dendrobe in the first to fifth embodiments, the quality detection methods for medicinal dendrobe in the first to fifth embodiments are as follows:
from the above table, the extraction rate of the quality detection method for medicinal dendrobium of the present invention is obviously improved, and the second embodiment is the best embodiment.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A quality detection method of medicinal dendrobium medicinal material is characterized by comprising the following steps:
s1: obtaining a medicinal dendrobium medicinal material sample, crushing the medicinal dendrobium medicinal material sample to prepare dendrobium powder, then 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 the 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 ether and 50-60 ml of propanol, mixing to prepare a first solution, pouring the first solution into a stirring container, adding the weighed dendrobe powder into the first solution, stirring until the dendrobe powder is completely dissolved in the mixed solution, pouring the mixed solution into ultrasonic extraction equipment, and drying the extract after extraction to obtain a primary extracting solution;
s3: adding a second solution into the primary extracting solution, wherein the second solution consists of 150-200 ml of 10% ammonia water, 15-25 g of sodium hydroxide and 5-15 g of potassium hydrogen phthalate, uniformly stirring, controlling the stirring time to be 10-15 minutes, carrying out rotary drying at the temperature of 60-65 ℃, then adding 50ml of a third solution, uniformly stirring, wherein the third solution is a mixed solution of trichloromethane and methanol, hermetically standing for 30 minutes, and filtering the solution after standing to obtain a sample extract;
s4: obtaining a dendrobine-containing control sample, pouring the dendrobine-containing control sample into the prepared first solution, stirring, extracting by using ultrasonic extraction equipment, adding the prepared second solution, uniformly stirring, drying, adding the third solution, uniformly stirring, standing and filtering to obtain a comparative extracting solution;
s5: and (3) obtaining a sample extract and a comparison extract, respectively adding a bromokaliophenol 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, so that the quality of the medicinal dendrobium nobile material can be obtained.
2. The method of claim 1, wherein in step S1, the obtained sample of Dendrobium officinale is screened in advance to remove unqualified materials, and then washed and dried to obtain the sample.
3. The method of claim 1, wherein in step S1, when the sample of Dendrobium nobile Linn is pulverized, the sample is first crushed in a blade crusher and then ground in a grinding device.
4. The method for detecting the quality of the medicinal dendrobium nobile material according to claim 1, wherein the dendrobium nobile powder is added in S2, the stirring container is sealed, 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.
5. The method for detecting the quality of the medicinal dendrobium nobile material according to claim 1, wherein in S2, the ultrasonic frequency is controlled to be 28 KHz-30 KHz, the power of the ultrasonic extraction equipment is controlled to be 400W-450W, and the extraction time is controlled to be 45 minutes-60 minutes.
6. The method for detecting the quality of the medicinal dendrobium nobile material as claimed in claim 1, wherein in S2, the extract is in a rotating state during drying, and the drying temperature is controlled at 60-65 ℃.
7. The method for detecting the quality of the medicinal dendrobium nobile material according to claim 1, wherein in S3, the chloroform and the methanol in the third solution are mixed according to the ratio of 9: 1.
8. The method for detecting the quality of the medicinal dendrobium nobile material according to claim 1, wherein in S3, the medicinal dendrobium nobile material is filtered by a micro-filtration membrane, and the pore size of the micro-filtration membrane is 0.50 micron.
9. The method of claim 1, wherein in S4, the dendrobine-containing control sample is selected from other types of dendrobe, and the extraction steps of the control sample are the same as those of the sample extract.
10. The method of claim 1, wherein in step S5, the weight of the obtained sample extract and the weight of the reference extract need to be the same, the addition amount of the green bromokaliophenol solution is 5ml, and 0.06% green bromokaliophenol solution is selected.
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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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| 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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