CN108593634A - The detection method of alkaloid in Chinese medicinal ingredients - Google Patents
The detection method of alkaloid in Chinese medicinal ingredients Download PDFInfo
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- CN108593634A CN108593634A CN201810437063.1A CN201810437063A CN108593634A CN 108593634 A CN108593634 A CN 108593634A CN 201810437063 A CN201810437063 A CN 201810437063A CN 108593634 A CN108593634 A CN 108593634A
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
Abstract
The present invention discloses a kind of detection method of alkaloid in Chinese medicinal ingredients, it includes the following steps, (1) takes sample comminution, and (2) are diluted with water, filter, (3) plus alcohol；(4) organic solvent is added；(5) aluminium oxide is added；(6) PH conditioning agents are added；(7) enrichment concentration will；(8) it measures：The present invention plays an important role the active ingredient in alkaloid in measurement drug, control traditional Chinese medicine quality, simultaneously, the quality good or not for weighing the stability and medicinal material of process of Chinese material medica preparation is contributed to reach the clinical application safely, effectively meaning with Chinese medicine for ensureing the quality of Chinese medicine.
Description
Technical field
The present invention relates to a kind of detection methods of alkaloid in Chinese medicine detection technique field more particularly to Chinese medicinal ingredients.
Background technology
Chinese medicine is acquired with Chinese traditional medicine theoretical direction, is processed, preparation, and illustration mechanism and guides clinical application,
In brief, Chinese medicine refers to just under instruction of Chinese Medicine theory, for preventing, treating, diagnosing the illness and make with rehabilitation and health care
Substance, Chinese medicine are mainly derived from crude drug and its processed goods, including autonomic drug, animal drugs, mineral drug and part chemistry, life
Tetramune class drug.Since Chinese medicine is in the majority with autonomic drug, therefore there is the saying of " all medicines are with grass for this "；But traditional Chinese medicine ingredients are complicated, production
Crude drug effect is not certain single component, and measuring certain, the active ingredient of flavour of a drug, active constituent have control traditional Chinese medicine quality simply
Important role, meanwhile, the quality good or not of stability and medicinal material for weighing process of Chinese material medica preparation, to ensure the matter of Chinese medicine
Amount reaches the clinical application safely, effectively meaning with Chinese medicine.
Invention content
It it is an object of the invention to overcome the deficiencies in the prior art, adapts to reality and needs, disclose and is given birth in a kind of Chinese medicinal ingredients
The detection method of alkaloids.
In order to achieve the object of the present invention, the technical solution adopted in the present invention is：
A kind of detection method of alkaloid in Chinese medicinal ingredients is disclosed, it is characterised in that：It includes the following steps：
(1) 50g sample comminutions, powder particle diameter to -100 mesh of 40 mesh are taken；
(2) it is diluted with water and using the strainer filtering of 100 mesh, removes the impurity in solution；
(3) impurity filtered out is crushed or is ground again；
(4) it is added after water dilution and equally uses the strainer filtering of 100 mesh；
(5) step (3), (4) are repeated up to free from admixture phenomenon in solution；
(6) solution in step (2), (4) is mixed；
(7) alcohol 10-20g is added and vibrates 30-90min in 30 DEG C -40 DEG C of water-bath；
(8) organic solvent 10-15g is added and in 50 DEG C -80 DEG C of stirred in water bath 10-20min；
(9) aluminium oxide 0.5-1.0g is added；
(10) PH conditioning agents are added, it is in free state to be adjusted to make for 7.5-9.0 the alkaloid in solution by PH；
(11) enrichment is concentrated the moisture evaporation in solution；
(12) solvent prepared by step (11) is respectively placed in tri- transparent test tubes of A, B, C；
(13) it measures：
Measure A：The secret potassium 0.5-1.0g of iodate will be added in A, stand 3-5min, then, ferric trichloride 0.5-1.0g is added
It stirs and stands 3-5min；
Measure B：The secret potassium 0.5-1.0g of iodate will be added in B, stand 3-5min, then, ninhydrin 0.5-1.0g is added and stirs
It mixes and stands 3-5min；；
Measure C：C is placed under ultraviolet and is irradiated.
Preferably, the water is distilled water.
Preferably, the alcohol is methanol, and the PH of the methanol is 6-7.
Preferably, the organic solvent is styrene or trichloroethanes.
Preferably, the PH of the aluminium oxide is 7.
The beneficial effects of the present invention are：
Each easily operated implementation of step in this method, for exhausted most Chinese medicines or Chinese medicine in the market, such as fiber crops in implementation
Huang, the rhizome of Chinese monkshood, the coptis, ginseng, vomiting nut etc. can be detected it, for measure active ingredient in drug in alkaloid,
Control traditional Chinese medicine quality play an important role, meanwhile, contribute to weigh process of Chinese material medica preparation stability and medicinal material it is quality
It is bad, for ensureing the quality of Chinese medicine, reach the clinical application safely, effectively meaning with Chinese medicine.
Specific implementation mode
With reference to embodiment, the present invention is further described：
Embodiment 1：In a kind of Chinese medicinal ingredients the detection method of alkaloid it include the following steps：
(1) 50g sample comminutions or grinding are taken, makes its grain size between -100 mesh of 40 mesh.
(2) it is diluted to liquid using distilled water (the distilled water slant acidity, PH is between 6.0-6.9) water, then uses 100
Purpose strainer filtering removes the impurity in solution.
(3) impurity filtered out in step (2) is crushed or is ground again.
(4) equally make to being added in step (3) after distilled water (the distilled water slant acidity, PH is between 6.0-6.9) dilutes
With the strainer filtering of 100 mesh.
(5) step (3), (4) are repeated up to free from admixture phenomenon in solution.
(6) solution in step (2), (4) is mixed.
(7) methanol (PH 6-7) 10-20g is added and vibrates 30-90min in 30 DEG C -40 DEG C of water-bath, methanol is added and promotees
So that alkaloid is reacted with methanol and be dissolved in solution, should avoid temperature is excessively high methanol transition volatilization is caused to cause to imitate in this step
The phenomenon that fruit reduces, and biogenic salt cannot be completely dissolved.
(8) styrene or trichloroethanes 10-15g is added and in 50 DEG C -80 DEG C of stirred in water bath 10-20min, alkaloid
It dissolves in styrene or trichloroethanes, by can further be fused alkaloid in this step.
(9) aluminium oxide 0.5-1.0g is added, with the flavones ingredient in Adsorption solution, to life when reducing late detection
The interference of alkaloids.
(10) PH conditioning agents are added, it is in free state to be adjusted to make for 7.5-9.0 the alkaloid in solution by PH.
(11) enrichment is concentrated the moisture evaporation in solution.
(12) solvent prepared by step (11) is respectively placed in tri- transparent test tubes of A, B, C.
(13) it measures：
Measure A：The secret potassium 0.5-1.0g of iodate being added in A, stands 3-5min, observation has precipitation to generate, while precipitating
Color changes (orange red), at this time the presence of preliminary proof alkaloid, then, ferric trichloride is added and (ferric trichloride is added
Color developing effect can be enhanced) 0.5-1.0g stirs and stands 3-5min, when color burn, highlight when can further prove that alkaloid is deposited
.
Measure B：The secret potassium 0.5-1.0g of iodate will be added in B, stands 3-5min, observation changes without phenomenon, and indenes three is added
Ketone 0.5-1.0g is stirred and is stood 3-5min；Observation color changes, and proves that the alkaloid in sample is hydrochloric acid Chinese ephedra at this time
Bases (ephedrine hydrochloride class does not react with ephedrine hydrochloride class).
Measure C：C is placed under ultraviolet and is irradiated, different colors occurs under ultraviolet light according to bases and is compared
To prove whether there is the presence of bases in sample.
Embodiment 2, place same as Example 1 repeat no more, the difference is that：
In step (2), distilled water PH is 6.0.
In step (7), the methanol 10g that PH is 6 is added and vibrates 30min in 30 DEG C of water-bath.
In step (8), styrene or trichloroethanes 10g is added and in 50 DEG C of stirred in water bath 10min.
In step (9), aluminium oxide 0.5g is added.
Embodiment 3, place same as Example 1 repeat no more, the difference is that：
In step (2), distilled water PH is 6.9.
In step (7), the methanol 20g that PH is 7 is added and vibrates 90min in 30 DEG C -40 DEG C of water-bath.
In step (8), styrene or trichloroethanes 115g is added and in 50 DEG C -80 DEG C of stirred in water bath 20min.
In step (9), aluminium oxide 1.0g is added.
Embodiment 4, place same as Example 1 repeat no more, the difference is that：
In step (2), distilled water PH is 6.5.
In step (7), the methanol 15g that PH is 6-7 is added and vibrates 50min in 35 DEG C of water-bath.
In step (8), styrene or trichloroethanes 13g is added and in 6080 DEG C of stirred in water bath 15min.
In step (9), aluminium oxide 0.8g is added.
To sum up, this method can be to exhausted most Chinese medicines or Chinese medicine in the market, such as Chinese ephedra, the rhizome of Chinese monkshood, the coptis, ginseng, Strychnos nux-vomica
Son etc. can be detected it, have for the active ingredient in alkaloid in measurement drug, control traditional Chinese medicine quality important
Effect, meanwhile, contribute to the quality good or not for weighing the stability and medicinal material of process of Chinese material medica preparation, for ensureing the quality of Chinese medicine,
Reach the clinical application safely, effectively meaning with Chinese medicine.
What the embodiment of the present invention was announced is preferred embodiment, and however, it is not limited to this, the ordinary skill people of this field
Member understands the spirit of the present invention easily according to above-described embodiment, and makes different amplification and variation, but as long as not departing from this
The spirit of invention, all within the scope of the present invention.
Claims (5)
1. the detection method of alkaloid in a kind of Chinese medicinal ingredients, it is characterised in that：It includes the following steps：
(1) 50g sample comminutions, powder particle diameter to -100 mesh of 40 mesh are taken；
(2) it is diluted with water and using the strainer filtering of 100 mesh, removes the impurity in solution；
(3) impurity filtered out is crushed or is ground again；
(4) it is added after water dilution and equally uses the strainer filtering of 100 mesh；
(5) step (3), (4) are repeated up to free from admixture phenomenon in solution；
(6) solution in step (2), (4) is mixed；
(7) alcohol 10-20g is added and vibrates 30-90min in 30 DEG C -40 DEG C of water-bath；
(8) organic solvent 10-15g is added and in 50 DEG C -80 DEG C of stirred in water bath 10-20min；
(9) aluminium oxide 0.5-1.0g is added；(with the flavones ingredient in Adsorption solution, reducing the interference to alkaloid)
(10) PH conditioning agents are added, it is in free state to be adjusted to make for 7.5-9.0 the alkaloid in solution by PH；
(11) enrichment is concentrated the moisture evaporation in solution；
(12) solvent prepared by step (11) is respectively placed in tri- transparent test tubes of A, B, C；
(13) it measures：
Measure A：The secret potassium 0.5-1.0g of iodate will be added in A, stand 3-5min, then, ferric trichloride 0.5-1.0g stirrings is added
And stand 3-5min；
Measure B：The secret potassium 0.5-1.0g of iodate will be added in B, stand 3-5min, then, ninhydrin 0.5-1.0g stirrings is added simultaneously
Stand 3-5min；；
Measure C：C is placed under ultraviolet and is irradiated.
2. the detection method of alkaloid in Chinese medicinal ingredients as described in claim 1, it is characterised in that：The water is distilled water.
3. the detection method of alkaloid in Chinese medicinal ingredients as described in claim 1, it is characterised in that：The alcohol is methanol, institute
The PH for stating methanol is 6-7.
4. the detection method of alkaloid in Chinese medicinal ingredients as described in claim 1, it is characterised in that：The organic solvent is benzene
Ethylene or trichloroethanes.
5. the detection method of alkaloid in Chinese medicinal ingredients as described in claim 1, it is characterised in that：The PH of the aluminium oxide is
7。
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1600777A (en) * | 2003-09-25 | 2005-03-30 | 中国科学院过程工程研究所 | New method for picking-up alkakoid of Chinese ephedra in large scale |
| CN1730480A (en) * | 2005-08-02 | 2006-02-08 | 山东轻工业学院 | Total coptis alkaloid preparation method |
| CN101011474A (en) * | 2007-02-08 | 2007-08-08 | 南昌弘益科技有限公司 | Limitary determination of traditional medicine aconitine containing radix aconiti kusnezoffii praeparata |
| CN101619105A (en) * | 2009-04-08 | 2010-01-06 | 黄宝生 | Process for extracting tea polysaccharide from tea leaf seed meal |
| CN103027946A (en) * | 2011-09-30 | 2013-04-10 | 北京因科瑞斯医药科技有限公司 | Method for extracting total alkaloids in semen strychni |
| CN106706626A (en) * | 2017-02-17 | 2017-05-24 | 西南民族大学 | Ingredient identification and antibacterial activity evaluation method of cliff honeysuckle |
-
2018
- 2018-05-09 CN CN201810437063.1A patent/CN108593634A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1600777A (en) * | 2003-09-25 | 2005-03-30 | 中国科学院过程工程研究所 | New method for picking-up alkakoid of Chinese ephedra in large scale |
| CN1730480A (en) * | 2005-08-02 | 2006-02-08 | 山东轻工业学院 | Total coptis alkaloid preparation method |
| CN101011474A (en) * | 2007-02-08 | 2007-08-08 | 南昌弘益科技有限公司 | Limitary determination of traditional medicine aconitine containing radix aconiti kusnezoffii praeparata |
| CN101619105A (en) * | 2009-04-08 | 2010-01-06 | 黄宝生 | Process for extracting tea polysaccharide from tea leaf seed meal |
| CN103027946A (en) * | 2011-09-30 | 2013-04-10 | 北京因科瑞斯医药科技有限公司 | Method for extracting total alkaloids in semen strychni |
| CN106706626A (en) * | 2017-02-17 | 2017-05-24 | 西南民族大学 | Ingredient identification and antibacterial activity evaluation method of cliff honeysuckle |
Non-Patent Citations (4)
| Title |
|---|
| CHENGGONGBA_..: "第十章生物碱", 《HTTPS://WWW.DOCIN.COM/P-327522679.HTML》 * |
| S4433318: "中成药中生物碱类成分的快速检验", 《HTTPS://WWW.DOCIN.COM/P-1592373839.HTML》 * |
| 田珊珊: "猕猴桃成熟过程中超微弱发光的研究", 《中国优秀硕士学位论文全文数据库 农业科技辑》 * |
| 知识百科: "介绍几种风味食品制作方法", 《资源节约和综合利用》 * |
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Application publication date: 20180928 |
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