CN109721583A - A kind of preparation method of aristolochic acid A and Aristolochic acid B C standard items - Google Patents
A kind of preparation method of aristolochic acid A and Aristolochic acid B C standard items Download PDFInfo
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Abstract
The present invention relates to separating and purifying technology field, in particular to a kind of preparation method of aristolochic acid A standard items and Aristolochic acid B C standard items.The present invention combines preparative high performance liquid chromatography, reverse polymerization filling adsorption means to isolate and purify to obtain aristolochic acid A and Aristolochic acid B C using dutchmanspipe root as raw material, using alcohol extracting, ethyl acetate extraction.Through detecting, the HPLC purity of two kinds of products 99% or more, can be used as quality monitoring of the standard items for Chinese medicine and its preparation containing aristolochic acid A and Aristolochic acid B C.Meanwhile the yield of aristolochic acid A standard items is 80%, the yield of Aristolochic acid B C standard items is 70%.The aristolochic acid A standard items and Aristolochic acid B C standard items purity is high, high income of preparation method preparation provided by the invention, simple process and low cost, the project output value is high, can be applied to industrialized production.
Description
Technical field
The present invention relates to the standard items of separating and purifying technology field more particularly to a kind of aristolochic acid A and Aristolochic acid B C
Preparation method.
Background technique
Aristolochic acid (Aristolochic acids, abbreviation AAs) is also referred to as Aristolochic acid, aristolochic acid or caulis akebiae
A prime, is a kind of nitro phenanthrene carboxylic acid, including aristolochic acid A, Aristolochic acid B C, aristolochic acid C and aristolochic acid D, have anticancer and
Anti-infective isoreactivity can be used for the infectious diseases such as bronchitis, tonsillitis, ephritis, prostatitis.Aristolochic acid is naturally deposited
It is in the aristolochiaceae plants such as Aristolochia (Aristolochia) and asarum (Asarum), according to related research, horse
Pocket bell platymiscium has more than 350 kinds, in China's Chinese traditional herbs, has tens of kinds of plant medicinal materials to contain Aristolochic Acid and horse pocket
Bell lactams ingredient is managed wherein included or once supervised by the Ministry of Public Health, national drug and food and medicine by " Chinese medicine pharmacopeia " in the past
Reason office etc. ratify medicinal medicinal material include birthwort, caulis aristologhiae manshuriensis, aristolochia fangchi, dutchmanspipe root, herba aristolochiae, berba aristolochiae mollissimae, cinnabar even etc., carefully
Pungent platymiscium mainly has Herba Asari and asarum sieboldii etc..
Currently, aristolochic acid substance is mainly used for the quality prison of above-mentioned medicinal material and the Chinese materia medica preparation containing above-mentioned medicinal material
Control.However, existing aristolochic acid A and Aristolochic acid B C standard items price and its valuableness, and purity is also inadequate, generally exists
95% or so, directly affect comprehensive, the system research that aristolochic acid quality controls in Chinese medicine.
Summary of the invention
In view of this, the purpose of the present invention is to provide the preparation sides of a kind of aristolochic acid A and the standard items of Aristolochic acid B C
Method.
In order to achieve the object of the present invention, the present invention adopts the following technical scheme:
The present invention provides the preparation method of a kind of aristolochic acid A standard items and Aristolochic acid B C standard items, including walks as follows
It is rapid:
Dutchmanspipe root is taken to crush, alcohol extracting, ethyl acetate layer is collected in ethyl acetate extraction, pure through preparative high performance liquid chromatography
Change, respectively obtains the sterling solution containing aristolochic acid A, Aristolochic acid B C；
The sterling solution is taken successively to be concentrated under reduced pressure respectively, upper reverse polymerization filling adsorption, the parsing of 90-95% alcohol,
After desorbed solution concentration, drying, aristolochic acid A standard items and Aristolochic acid B C standard items are obtained；
The chromatographic condition of the preparative high performance liquid chromatography are as follows: be 0.05- with volume fraction using acetonitrile as mobile phase A
0.2% acid solution is Mobile phase B, gradient elution.
Dutchmanspipe root is the drying of aristolochiaceae plant birthwort Aristolochia debilis Sieb.et Zucc.
Root, main component are aristolone, aristolochic acid, allantoin, debilic acid, magnoflorine etc..Dutchmanspipe root is as in one kind
Medicine medicinal material is worked hard, and is trembled with fear, is entered lung, stomach meridian.Tang Materia Medica: main accumulation.All scorchingly hot swollen, snake venom, water rub for mudding it, day three, four；
Treat malignant boil enlargement effect." vegetation is just square ": delivering, and removes wind.Cure mainly rheumatism paralysis, waist foot pain pain, traumatic injury；Chest and abdomen swelling and pain, acute filthy disease,
Enteritis diarrhea, hypertension, hernia, snake sting poison, carbuncle swells, furunculosis, pruitus or wet rotten etc..
The present invention is extracted in conjunction with preparative high performance liquid chromatography, reversely using dutchmanspipe root as raw material using alcohol extracting, ethyl acetate
Polymerization filling absorption means isolate and purify to obtain aristolochic acid A and Aristolochic acid B C.Through detecting, the purity of two kinds of product HPLC is equal
99% or more, quality monitoring of the standard items for Chinese medicine and its preparation containing aristolochic acid A and Aristolochic acid B C can be used as.
It is computed, the yield of aristolochic acid A standard items is 80%, and the yield of Aristolochic acid B C standard items is 70%.System provided by the invention
The aristolochic acid A standard items and Aristolochic acid B C standard items purity is high, high income of Preparation Method preparation, simple process and low cost, item
The mesh output value is high, can be applied to industrialized production.
In some embodiments, the alcohol extracting be 50%-100% with volume fraction methanol or volume fraction be
The ethyl alcohol of 50%-100% extracts, and the method for the alcohol extracting is refluxing extraction, ultrasonic extraction or seepage pressure effects；The alcohol extracting
Number be 3-6 time, the time extracted every time be 1-2 hours.
In some embodiments, the number of ethyl acetate extraction is 3-6 times, and the time extracted every time is 20~30min.
It in some embodiments, further include being concentrated under reduced pressure after the alcohol extracting, before ethyl acetate extraction
Step, the temperature of the reduced pressure are 50-70 DEG C.
The present invention further includes the steps that carrying out being concentrated into medicinal extract to ethyl acetate layer after collecting ethyl acetate layer.Then it uses
Preparative high performance liquid chromatography purifies the medicinal extract after concentration, respectively obtains the sterling containing aristolochic acid A, Aristolochic acid B C
Solution.Wherein, in preparative high performance liquid chromatography:
Acid solution is the aqueous solution of formic acid, acetic acid or phosphoric acid.
Isocratic elution program is 0~35min, and acetonitrile percentage by volume is 50~70%.
Detection wavelength is 260nm or 315nm.
The flow velocity of mobile phase is 1.0mL/min.
In some specific embodiments, isocratic elution program is 0~35min, and acetonitrile percentage by volume is 60%.
The chromatographic column that high performance liquid chromatography uses is AgilentC18, having a size of 100cm × (10-15) cm, 10-50 μm；
The column temperature of the chromatographic column is 25 DEG C.
Obtain containing aristolochic acid A, Aristolochic acid B C sterling solution after, respectively by containing aristolochic acid A, Aristolochic acid B C it is pure
Product solution is successively concentrated under reduced pressure, upper reverse polymerization filling adsorption, the parsing of 90-95% alcohol, and desorbed solution concentration, drying obtain horse
Pocket bell acid A standard items and Aristolochic acid B C standard items.
In some specific embodiments, the sterling solution containing aristolochic acid A is taken successively to be concentrated under reduced pressure, it is upper reversed poly-
Filling adsorption, the parsing of 90-95% alcohol are closed, desorbed solution concentration, drying obtain aristolochic acid A standard items.In other specific embodiment parties
In case, the sterling solution containing Aristolochic acid B C is taken successively to be concentrated under reduced pressure, upper reverse polymerization filling adsorption, 90-95% alcoholysis
Analysis, desorbed solution concentration, drying, obtains Aristolochic acid B C standard items.
In some embodiments, the temperature that the sterling solution is concentrated under reduced pressure is 50-70 DEG C.
In some embodiments, the reverse polymerization filler includes macroreticular resin AB-8, macroreticular resin D-101, polyamides
Amine or NM series chromatograph packing material.
The aristolochic acid A standard items and the preparation method of Aristolochic acid B C standard items provided by the invention of preparing include following step
It is rapid: take dutchmanspipe root to crush, alcohol extracting, ethyl acetate extraction is collected ethyl acetate layer, is purified through preparative high performance liquid chromatography, point
The sterling solution containing aristolochic acid A, Aristolochic acid B C is not obtained；The sterling solution is taken successively to be concentrated under reduced pressure respectively, it is upper anti-
It is adsorbed to polymerization filling, the parsing of 90-95% alcohol obtains aristolochic acid A standard items and Aristolochic acid B C after desorbed solution concentration, drying
Standard items；The chromatographic condition of the preparative high performance liquid chromatography are as follows: be 0.05- with volume fraction using acetonitrile as mobile phase A
0.2% acid solution is Mobile phase B, isocratic elution.
The product that the present invention is prepared is accredited as aristolochic acid A and Aristolochic acid B C through nuclear magnetic resonance, and HPLC purity exists
99% or more, therefore can be used as quality of the standard items for Chinese medicine and its preparation containing aristolochic acid A and Aristolochic acid B C and supervise
Control.Meanwhile the yield for being computed aristolochic acid A standard items is 80%, the yield of Aristolochic acid B C standard items is 70%.This method
The aristolochic acid A standard items and Aristolochic acid B C standard items purity is high, high income of preparation, simple process and low cost, the project output value
Height can be applied to industrialized production.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described.
Fig. 1 shows that ethyl acetate layer concentrated extract prepares test map online in the embodiment of the present invention 1；
Fig. 2 shows the nuclear magnetic resonance map of aristolochic acid A prepared by the embodiment of the present invention 1；
Fig. 3 shows the nuclear magnetic resonance map of Aristolochic acid B C prepared by the embodiment of the present invention 1；
Fig. 4 shows the HPLC map of aristolochic acid A prepared by the embodiment of the present invention 1；
Fig. 5 shows the HPLC map of Aristolochic acid B C prepared by the embodiment of the present invention 1.
Specific embodiment
The invention discloses the preparation method of a kind of aristolochic acid A and the standard items of Aristolochic acid B C, those skilled in the art
Present disclosure can be used for reference, realization of process parameters is suitably modified.In particular, it should be pointed out that all similar substitutions and modifications pair
It is it will be apparent that they are considered as being included in the present invention for those skilled in the art.Method and application of the invention is
Through being described by preferred embodiment, related personnel obviously can not depart from the content of present invention, in spirit and scope to this
Methods and applications described in text are modified or appropriate changes and combinations, carry out implementation and application the technology of the present invention.
To the explanation of the disclosed embodiments, enable those skilled in the art to implement or use the present invention.To this
A variety of modifications of a little embodiments will be readily apparent to those skilled in the art, as defined herein general
Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will not
It can be intended to be limited to the embodiments shown herein, and be to fit to consistent with the principles and novel features disclosed in this article
Widest scope.
The test material that the present invention uses is all common commercially available product, can all be bought in market.
Below with reference to embodiment, the present invention is further explained:
The preparation method of the present invention of embodiment 1
(1) it extracts
Dutchmanspipe root medicinal material is taken, is crushed, refluxing extraction is carried out with the ethyl alcohol that concentration is 80%, extracts 5 times, extract 1.5 every time
Hour, after extracting thoroughly, merge all extracting solutions, be concentrated under reduced pressure in 65 DEG C, be concentrated into no alcohol, collects concentrate, it is spare.
(2) enrichment pretreatment
Above-mentioned concentrate is diluted with water, and is then extracted with isometric ethyl acetate, extracts 5 times, combined ethyl acetate
Layer, is concentrated into medicinal extract, and water layer abandons.Ethyl acetate layer is total organic acids class position.
(3) preparative high-performance liquid chromatographic
The medicinal extract for taking step (2) is purified by preparative efficient liquid phase, is examined according to aristolochic acid A and Aristolochic acid B C
The corresponding bands of a spectrum that mapping composes (as shown in Figure 1) collect solution, wherein the retention time of Aristolochic acid B C bands of a spectrum is 20-25min, horse
The retention time of pocket bell acid A is 28-38min, obtains the solution of sterling containing aristolochic acid A and the sterling solution containing Aristolochic acid B C.
(4) reverse polymerization filling adsorption
The solution of sterling containing aristolochic acid A and the sterling solution containing Aristolochic acid B C are taken respectively, are successively concentrated under reduced pressure, on
Reverse polymerization filling adsorption, the parsing of 90% alcohol after desorbed solution concentration, drying, respectively obtain two kinds of powdered rubbers, and one kind is yellow
Powder, one kind are red-brown powder, identify that yellow powder is aristolochic acid A, molecular formula C through nuclear magnetic resonance17H11NO7, structure
Shown in formula I.Red-brown powder is Aristolochic acid B C, molecular formula C16H9NO6, structure is as shown in Formula II.The core of aristolochic acid A
Magnetic resonance map is shown in that Fig. 2, the nuclear magnetic resonance map of Aristolochic acid B C are shown in Fig. 3.
The above-mentioned aristolochic acid A being prepared and Aristolochic acid B C is taken to carry out the detection of Quality Control chromatography.Wherein, HPLC detector bar
Part are as follows:
Chromatographic column AgilentC18 (250nm × 4.6nm, 5 μm), is 0.05- with volume fraction using acetonitrile as mobile phase A
0.2% formic acid or phosphoric acid solution is Mobile phase B, gradient elution.Flow velocity 1.0ml/min；25 DEG C of column temperature；Detection wavelength is
260nm or 315nm；Wherein, gradient elution program are as follows: 0-35min, acetonitrile volume fraction is by 30% to 53%.
The HPLC map of aristolochic acid A is shown in that Fig. 4, the HPLC map of Aristolochic acid B C are shown in Fig. 5, and characteristic peak data is shown in Table 1~2.
By Tables 1 and 2 it is found that the HPLC purity of aristolochic acid A (No. 14 peaks) is 99.06%, the HPLC of Aristolochic acid B C (No. 4 peaks) is pure
Degree is 99.33%, and the purity of two kinds of products can be used as standard items for containing aristolochic acid A and horse pocket 99% or more
The quality monitoring of the Chinese medicine and its preparation of bell acid B.
The yield of preparation method aristolochic acid A/B of the present invention is calculated according to the following formula:
Aristolochic acid A/B yield=(aristolochic acid A/B content made from every kg dutchmanspipe root)/(horse in every kg dutchmanspipe root
The theoretical content of pocket bell acid A/B)
It is computed, the yield of aristolochic acid A standard items prepared by preparation method of the present invention is 82%, Aristolochic acid B C standard
The yield of product is 72%.
The chromatographic data of 1 aristolochic acid A of table
The chromatographic data of 2 aristolochic acid A of table
Embodiment 2
(1) it extracts
Dutchmanspipe root medicinal material is taken, is crushed, is that 50% methanol carries out ultrasonic extraction with concentration, extracts 3 times, extract 1 hour every time,
After extracting thoroughly, merge all extracting solutions, be concentrated under reduced pressure in 70 DEG C, be concentrated into no alcohol, collects concentrate, it is spare.
(2) enrichment pretreatment
Above-mentioned concentrate is diluted with water, and is then extracted with isometric ethyl acetate, extracts 5 times, combined ethyl acetate
Layer, is concentrated into medicinal extract, and water layer abandons.Ethyl acetate layer is total organic acids class position.
(3) preparative high-performance liquid chromatographic
The medicinal extract for taking step (2) is purified by preparative efficient liquid phase, is examined according to aristolochic acid A and Aristolochic acid B C
The corresponding bands of a spectrum of mapping spectrum collect solution, wherein the retention time of Aristolochic acid B C bands of a spectrum is 20-25min, the guarantor of aristolochic acid A
Staying the time is 28-38min, obtains the solution of sterling containing aristolochic acid A and the sterling solution containing Aristolochic acid B C.
(4) reverse polymerization filling adsorption
The solution of sterling containing aristolochic acid A and the sterling solution containing Aristolochic acid B C are taken respectively, are successively concentrated under reduced pressure, on
Reverse polymerization filling adsorption, the parsing of 90% alcohol after desorbed solution concentration, drying, respectively obtain two kinds of powdered rubbers, and one kind is yellow
Powder, one kind are red-brown powder, are followed successively by aristolochic acid A and Aristolochic acid B C through nuclear magnetic resonance identification.
The purity of aristolochic acid A and Aristolochic acid B C is detected according to the Quality Control chromatographic condition of embodiment 1, and according to
The method calculated yield of embodiment 1.The results show that the HPLC purity of aristolochic acid A is 99.0%, the HPLC of Aristolochic acid B C is pure
Degree is 99.1%, and the yield of aristolochic acid A standard items is 81%, and the yield of Aristolochic acid B C standard items is 71%.
Embodiment 3
(1) it extracts
Dutchmanspipe root medicinal material is taken, is crushed, is that 80% methanol carries out ultrasonic extraction with concentration, extracts 3 times, extract 1 hour every time,
After extracting thoroughly, merge all extracting solutions, be concentrated under reduced pressure in 50 DEG C, be concentrated into no alcohol, collects concentrate, it is spare.
(2) enrichment pretreatment
Above-mentioned concentrate is diluted with water, and is then extracted with isometric ethyl acetate, extracts 5 times, combined ethyl acetate
Layer, is concentrated into medicinal extract, and water layer abandons.Ethyl acetate layer is total organic acids class position.
(3) preparative high-performance liquid chromatographic
The medicinal extract for taking step (2) is purified by preparative efficient liquid phase, is examined according to aristolochic acid A and Aristolochic acid B C
The corresponding bands of a spectrum of mapping spectrum collect solution, wherein the retention time of Aristolochic acid B C bands of a spectrum is 20-25min, the guarantor of aristolochic acid A
Staying the time is 28-38min, obtains the solution of sterling containing aristolochic acid A and the sterling solution containing Aristolochic acid B C.
(4) reverse polymerization filling adsorption
The solution of sterling containing aristolochic acid A and the sterling solution containing Aristolochic acid B C are taken respectively, are successively concentrated under reduced pressure, on
Reverse polymerization filling adsorption, the parsing of 95% alcohol after desorbed solution concentration, drying, respectively obtain two kinds of powdered rubbers, and one kind is yellow
Powder, one kind are red-brown powder, are followed successively by aristolochic acid A and Aristolochic acid B C through nuclear magnetic resonance identification.
The purity of aristolochic acid A and Aristolochic acid B C is detected according to the Quality Control chromatographic condition of embodiment 1, and according to
The method calculated yield of embodiment 1.The results show that the HPLC purity of aristolochic acid A is 99.5%, the HPLC of Aristolochic acid B C is pure
Degree is 99.6%, and the yield of aristolochic acid A standard items is 83%, and the yield of Aristolochic acid B C standard items is 72%.
Embodiment 4
(1) it extracts
Dutchmanspipe root medicinal material is taken, is crushed, is that 50% ethyl alcohol carries out ultrasonic extraction with concentration, extracts 3 times, extract 1 hour every time,
After extracting thoroughly, merge all extracting solutions, be concentrated under reduced pressure in 60 DEG C, be concentrated into no alcohol, collects concentrate, it is spare.
(2) enrichment pretreatment
Above-mentioned concentrate is diluted with water, and is then extracted with isometric ethyl acetate, extracts 5 times, combined ethyl acetate
Layer, is concentrated into medicinal extract, and water layer abandons.Ethyl acetate layer is total organic acids class position.
(3) preparative high-performance liquid chromatographic
The medicinal extract for taking step (2) is purified by preparative efficient liquid phase, is examined according to aristolochic acid A and Aristolochic acid B C
The corresponding bands of a spectrum of mapping spectrum collect solution, wherein the retention time of Aristolochic acid B C bands of a spectrum is 20-25min, the guarantor of aristolochic acid A
Staying the time is 28-38min, obtains the solution of sterling containing aristolochic acid A and the sterling solution containing Aristolochic acid B C.
(4) reverse polymerization filling adsorption
The solution of sterling containing aristolochic acid A and the sterling solution containing Aristolochic acid B C are taken respectively, are successively concentrated under reduced pressure, on
Reverse polymerization filling adsorption, the parsing of 95% alcohol after desorbed solution concentration, drying, respectively obtain two kinds of powdered rubbers, and one kind is yellow
Powder, one kind are red-brown powder, are followed successively by aristolochic acid A and Aristolochic acid B C through nuclear magnetic resonance identification.
The purity of aristolochic acid A and Aristolochic acid B C is detected according to the Quality Control chromatographic condition of embodiment 1, and according to
The method calculated yield of embodiment 1.The results show that the HPLC purity of aristolochic acid A is 99.3%, the HPLC of Aristolochic acid B C is pure
Degree is 99.3%, and the yield of aristolochic acid A standard items is 80%, and the yield of Aristolochic acid B C standard items is 70%.
Comparative example 1
(1) it extracts
Dutchmanspipe root medicinal material is taken, is crushed, is that 40% ethyl alcohol carries out ultrasonic extraction with concentration, extracts 3 times, extract 1 hour every time,
After extracting thoroughly, merge all extracting solutions, be concentrated under reduced pressure in 60 DEG C, be concentrated into no alcohol, collects concentrate, it is spare.
(2) enrichment pretreatment
Above-mentioned concentrate is diluted with water, and is then extracted with isometric ethyl acetate, extracts 3 times, combined ethyl acetate
Layer, is concentrated into medicinal extract, and water layer abandons.Ethyl acetate layer is total organic acids class position.
(3) preparative high-performance liquid chromatographic
The ethyl acetate layer for taking step (2) is purified by preparative efficient liquid phase, preparation condition select with methanol for
Mobile phase A, using distilled water solution as Mobile phase B, isocratic elution, elution program is 0~35min, and methanol percentage by volume is 50
~95%, solution is collected according to aristolochic acid A and the corresponding bands of a spectrum of Aristolochic acid B C test map, wherein Aristolochic acid B C bands of a spectrum
Retention time be 10-14min, the retention time of aristolochic acid A is 18-25min, obtain the solution of sterling containing aristolochic acid A with
Sterling solution containing Aristolochic acid B C.
(4) reverse polymerization filling adsorption
The solution of sterling containing aristolochic acid A and the sterling solution containing Aristolochic acid B C are taken respectively, are successively concentrated under reduced pressure, on
Reverse polymerization filling adsorption, the parsing of 80% alcohol after desorbed solution concentration, drying, respectively obtain two kinds of powdered rubbers, and one kind is yellow
Powder, one kind are red-brown powder, are followed successively by aristolochic acid A and Aristolochic acid B C through nuclear magnetic resonance identification.
The purity of aristolochic acid A and Aristolochic acid B C is detected according to the Quality Control chromatographic condition of embodiment 1, and according to
The method calculated yield of embodiment 1.The results show that the HPLC purity of aristolochic acid A is 99.0%, the HPLC of Aristolochic acid B C is pure
Degree is 99.0%, and the yield of aristolochic acid A standard items is 55%, and the yield of Aristolochic acid B C standard items is 45%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of aristolochic acid A standard items and Aristolochic acid B C standard items, which comprises the steps of:
Dutchmanspipe root is taken to crush, alcohol extracting, ethyl acetate extraction collects ethyl acetate layer, purifies, obtain through preparative high performance liquid chromatography
To the sterling solution containing aristolochic acid A and the sterling solution containing Aristolochic acid B C；
The sterling solution is taken successively to be concentrated under reduced pressure respectively, upper reverse polymerization filling adsorption, the parsing of 90-95% alcohol, parsing
After liquid concentration, drying, aristolochic acid A standard items and Aristolochic acid B C standard items are obtained；
The chromatographic condition of the preparative high performance liquid chromatography are as follows: be 0.05-0.2% with volume fraction using acetonitrile as mobile phase A
Acid solution be Mobile phase B, isocratic elution.
2. according to right want 1 described in preparation method, which is characterized in that the acid solution is the aqueous solution of formic acid or phosphoric acid.
3. according to right want 1 described in preparation method, which is characterized in that the isocratic elution program be 0~35min, acetonitrile body
Product is 50~70%.
4. according to right want 1 described in preparation method, which is characterized in that the Detection wavelength of the preparative high performance liquid chromatography is
260nm or 315nm.
5. according to right want 1 described in preparation method, which is characterized in that the flow velocity of the mobile phase be 1.0mL/min.
6. according to right want 1 described in preparation method, which is characterized in that the chromatographic column that the preparative high performance liquid chromatography uses
For AgilentC18, the column temperature of the chromatographic column is 25 DEG C.
7. according to right want 1 described in preparation method, which is characterized in that the alcohol drawings volume fraction be 50%-100% first
The ethyl alcohol that alcohol or volume fraction are 50%-100% extracts；The method of the alcohol extracting is refluxing extraction, ultrasonic extraction or infiltration
It filters extraction；The number of the alcohol extracting is 3-6 times, and the time extracted every time is 1-2 hours.
8. according to right want 1 described in preparation method, which is characterized in that after the alcohol extracting, the ethyl acetate extract it
Before further include the steps that being concentrated under reduced pressure, the temperature of the reduced pressure is 50-70 DEG C.
9. according to right want 1 described in preparation method, which is characterized in that the reverse polymerization filler include macroreticular resin AB-8,
Macroreticular resin D-101, polyamide or NM series chromatograph packing material.
10. according to right want 1 described in preparation method, which is characterized in that the number of the extraction be 3-6 times, extract every time
Time is 20~30min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117147738A (en) * | 2023-10-31 | 2023-12-01 | 吉林市双士药业有限公司 | Method for detecting aristolochic acid I in refreshment and reconstruction pill |
| CN117147738B (en) * | 2023-10-31 | 2024-02-27 | 吉林市双士药业有限公司 | Method for detecting aristolochic acid I in refreshment and reconstruction pill |
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