CN105687675A - Method for extracting peimine and peiminine from Fritillaria thunbergii - Google Patents
Method for extracting peimine and peiminine from Fritillaria thunbergii Download PDFInfo
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- CN105687675A CN105687675A CN201610234659.2A CN201610234659A CN105687675A CN 105687675 A CN105687675 A CN 105687675A CN 201610234659 A CN201610234659 A CN 201610234659A CN 105687675 A CN105687675 A CN 105687675A
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- Prior art keywords
- peiminine
- peimine
- bulbus fritillariae
- extracting
- fritillariae thunbergii
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8966—Fritillaria, e.g. checker lily or mission bells
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J71/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
- C07J71/0036—Nitrogen-containing hetero ring
- C07J71/0042—Nitrogen only
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Alternative & Traditional Medicine (AREA)
- Epidemiology (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
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- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Botany (AREA)
- Animal Behavior & Ethology (AREA)
- Biotechnology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Engineering & Computer Science (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for extracting peimine and peiminine from Fritillaria thunbergii. The method includes the steps of firstly, grinding the Fritillaria thunbergii and sieving; secondly, weighing, by weight, 1 part of Fritillaria thunbergii powder and 1 part of diatomite with mixing uniformly for standby use; thirdly, after uniform mixing, adding an appropriate quantity of diatomite into an extraction pond with a prearranged filtering membrane to enable the diatomite to reach a pond mouth of the extraction pond, covering the extraction pond for static extraction and obtaining extraction liquor after extraction is terminated. The method for extracting the peimine and the peiminine from the Fritillaria thunbergii is simple to operate and high in extraction rate.
Description
Technical field
The present invention relates to test in laboratory field, particularly the extracting method of peimine, peiminine in a kind of Bulbus Fritillariae Thunbergii。
Background technology
Pharmacopeia in 2010 have recorded extracts the extracting method of peimine, peiminine in Bulbus Fritillariae Thunbergii: take this product powder (crossing No. four sieves) about 2g, accurately weighed, put in flask, add strong ammonia solution 4ml and infiltrate 1 hour, the accurate mixed solution 40ml adding chloroform-methanol (4:1), weighed weight, mixing, put in 80 DEG C of water-baths and be heated to reflux 2 hours, let cool, weighed weight again, adds above-mentioned mixed solution and supplies the weight of less loss, filters。Precision measures subsequent filtrate 10ml, puts in evaporating dish and is evaporated, and residue adds methanol to be made dissolving and is transferred in 2ml measuring bottle, adds methanol to scale, shakes up, to obtain final product。
The method operating process of pharmacopeia is complicated, and the operant skill of operator is required height。
Summary of the invention
It is an object of the invention to provide the extracting method of peimine, peiminine in a kind of Bulbus Fritillariae Thunbergii, the method is simple to operate, and extraction efficiency is high。
Technical scheme provided by the invention is: the extracting method of peimine, peiminine in a kind of Bulbus Fritillariae Thunbergii, comprises the following steps:
Step 1: after Bulbus Fritillariae Thunbergii is pulverized, sieve；
Step 2: weigh 1 weight portion Bulbus Fritillariae Thunbergii powder, mix homogeneously stand-by with 1 weight portion kieselguhr；
Step 3: in the abstraction pool putting filter membrane in advance well, adds appropriate kieselguhr to the Chi Kou reaching abstraction pool after mix homogeneously；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is percent by volume 75% ethanol；Extraction temperature 80 DEG C；Static extracting time 3min；Flush volume 60%；Quiet cycle number of times 2 times。
In above-mentioned Bulbus Fritillariae Thunbergii in the extracting method of peimine, peiminine, the volume of described abstraction pool is 10ml。
In above-mentioned Bulbus Fritillariae Thunbergii in the extracting method of peimine, peiminine, the pressure of described static extracting is 1500psi。
In above-mentioned Bulbus Fritillariae Thunbergii in the extracting method of peimine, peiminine, the purge time of described static extracting is 100s。
In above-mentioned Bulbus Fritillariae Thunbergii in the extracting method of peimine, peiminine, step 2 is particularly as follows: by extract centrifugal 3min when 15000r/min, take supernatant。
In above-mentioned Bulbus Fritillariae Thunbergii in the extracting method of peimine, peiminine, the instrument that described ASE extraction adopts is ASE350 Accelerate solvent extraction instrument。
The present invention is after adopting technique scheme, and it has the beneficial effect that
The detection method of the present invention is simple to operate, and precision is consistent with the precision of official method, reproducible。
Accompanying drawing explanation
Fig. 1 is the rectangular plots of the chromatography validation verification of peimine in the present invention；
Fig. 2 is the rectangular plots of the chromatography validation verification of peiminine in the present invention；
Fig. 3 is the chromatogram of the peimine reference substance of the present invention, peiminine reference substance；
Fig. 4 is the extraction of the present invention and method of testing obtains chromatogram。
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is described in further detail, but does not constitute any limitation of the invention。
Embodiment 1:
Size-reduced for Bulbus Fritillariae Thunbergii machine is pulverized, excessively No. four sieves, about 1g, accurately weighed, mix homogeneously with 1g kieselguhr, stand-by, it is moved into and put glass fiber filter in advance wellAdding proper amount of silicon diatomaceous earth in 10ml abstraction pool, jolting so as to Chi Kou in the same horizontal line, tightens abstraction pool upper cover gently。After extraction terminates, extract being shifted in 25ml volumetric flask, with methanol dilution to scale, under 15000r/min, centrifugal 3min, takes supernatant, enters LC and measures。
Extraction conditions (see table 1) is:
Table 1
Analysis method is LC liquid chromatography, liquid-phase chromatographic analysis condition:
A) the double; two ternary liquid phase (U-3000) of instrument: Thermo
B) chromatographic column: ThermoSyncronisC183*100mm3um, i.e. carbon 18 chromatographic column, length 100mm, diameter 3mm, particle diameter 3 microns；
C) column temperature: 40 DEG C
D) flow velocity: 0.5mL/min
E) mobile phase: acetonitrile-water-diethylamine, volume ratio 70:30:0.03
F) detection wavelength: evaporative light scattering detector。
Chromatography validation verification:
Take peimine reference substance, peiminine reference substance in right amount, accurately weighed, add methanol and make every 1ml mixed solution containing peimine 0.2mg, peiminine 0.15mg, obtain peimine reference substance, peiminine reference substance。
Take peimine reference substance, peiminine reference substance in right amount, accurately weighed, add methanol and make every 1ml mixed solution containing peimine 0.1791mg, peiminine 0.1240mg, to obtain final product。Then precision draws this solution 0.2 μ l, 0.5 μ l, 0.8 μ l, 1 μ l, 1.5 μ l, 2 μ l entrance LC mensuration respectively, and measures according to said method, the results detailed in Table 2-1, table 2-2。Accompanying drawing 1 is corresponding with table 2-1, and accompanying drawing 2 is corresponding with table 2-2, and the abscissa indicated concentration of accompanying drawing 1 and accompanying drawing 2, vertical coordinate represents peak area。Accompanying drawing 3 is the chromatogram adopting above-mentioned LC liquid chromatography for measuring of peimine reference substance, peiminine reference substance。
Table 2-1 (peimine linear relationship)
Table 2-2 (peiminine linear relationship)
The repeatability checking of the extracting process of 1.1 embodiments 1:
Take sample (lot number: the 150827) 1.0g of identical lot number, totally 4 parts, accurately weighed, extracting need testing solution by ASE extracting method, sample size is 3 μ L, with above-mentioned chromatographic condition parallel test, recording the content of peimine in sample is 2.54% in Table 3-1, RSD；Recording the content of peiminine in sample is 2.12% in Table 3-2, RSD；Test shows that ASE extracting method repeatability is good, the results detailed in Table 3-1, table 3-2
Table 3-1
Table 3-2
The degree of accuracy test of the extracting process of 1.2 embodiments 1
Bulbus Fritillariae Thunbergii is extracted by the extracting process adopting the ASE extracting process of embodiment 1 and pharmacopeia, and Bulbus Fritillariae Thunbergii is 4 batches, lot number respectively 1510111,151102,150827,150618；
The ASE extracting process of the embodiment 1 Bulbus Fritillariae Thunbergii parallel testing twice to same batch, respectively ASE1 and ASE2 represents。
Fig. 4 is the chromatogram that sample 150827 obtains according to ASE extracting process and LC liquid chromatography test (ASE2) of the present invention。
Concrete test result is shown in table 4 below；
Table 4
The above-described presently preferred embodiments of the present invention that is only, all any amendment, equivalent replacement and improvement etc. made within the scope of the spirit and principles in the present invention, should be included within protection scope of the present invention。
Claims (6)
1. the extracting method of peimine, peiminine in a Bulbus Fritillariae Thunbergii, it is characterised in that comprise the following steps:
Step 1: after Bulbus Fritillariae Thunbergii is pulverized, sieve；
Step 2: weigh 1 weight portion Bulbus Fritillariae Thunbergii powder, mix homogeneously stand-by with 1 weight portion kieselguhr；
Step 3: in the abstraction pool putting filter membrane in advance well, adds appropriate kieselguhr to the Chi Kou reaching abstraction pool after mix homogeneously；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is percent by volume 75% ethanol；Extraction temperature 80 DEG C；Static extracting time 3min；Flush volume 60%；Quiet cycle number of times 2 times。
2. the extracting method of peimine, peiminine in Bulbus Fritillariae Thunbergii according to claim 2, it is characterised in that the volume of described abstraction pool is 10ml。
3. the extracting method of peimine, peiminine in Bulbus Fritillariae Thunbergii according to claim 2, it is characterised in that the pressure of described static extracting is 1500psi。
4. the extracting method of peimine, peiminine in Bulbus Fritillariae Thunbergii according to claim 2, it is characterised in that the purge time of described static extracting is 100s。
5. the extracting method of peimine, peiminine in Bulbus Fritillariae Thunbergii according to claim 1, it is characterised in that step 2 is particularly as follows: by extract centrifugal 3min when 15000r/min, take supernatant。
6. the extracting method of peimine, peiminine in Bulbus Fritillariae Thunbergii according to claim 1, it is characterised in that the instrument that described ASE extraction adopts is ASE350 Accelerate solvent extraction instrument。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610234659.2A CN105687675A (en) | 2016-04-15 | 2016-04-15 | Method for extracting peimine and peiminine from Fritillaria thunbergii |
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| CN201610234659.2A CN105687675A (en) | 2016-04-15 | 2016-04-15 | Method for extracting peimine and peiminine from Fritillaria thunbergii |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106885862A (en) * | 2017-04-13 | 2017-06-23 | 广西壮族自治区梧州食品药品检验所 | A kind of ASE HPLC methods determine peimine, the method for the content of Peiminine in fritillaria thunbergii |
| CN106928115A (en) * | 2017-03-29 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE methods extract stachydrine hydrochloride in motherwort |
| CN112147243A (en) * | 2020-08-26 | 2020-12-29 | 浙江省人民医院 | Detection method for simultaneously determining multiple active ingredients in lung-clearing medicament |
| CN115372501A (en) * | 2022-07-27 | 2022-11-22 | 广州科曼生物科技有限公司 | Thunberg fritillary bulb or Hubei fritillary bulb contrast extract and preparation method and application thereof |
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| CN104407064A (en) * | 2014-10-22 | 2015-03-11 | 浙江康恩贝制药股份有限公司 | Fritillaria medicinal material identification and content determination method |
| CN104876988A (en) * | 2015-05-12 | 2015-09-02 | 广西壮族自治区梧州食品药品检验所 | Method for extracting linarin from wild chrysanthemum flower |
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2016
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| CN104407064A (en) * | 2014-10-22 | 2015-03-11 | 浙江康恩贝制药股份有限公司 | Fritillaria medicinal material identification and content determination method |
| CN104876988A (en) * | 2015-05-12 | 2015-09-02 | 广西壮族自治区梧州食品药品检验所 | Method for extracting linarin from wild chrysanthemum flower |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928115A (en) * | 2017-03-29 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE methods extract stachydrine hydrochloride in motherwort |
| CN106885862A (en) * | 2017-04-13 | 2017-06-23 | 广西壮族自治区梧州食品药品检验所 | A kind of ASE HPLC methods determine peimine, the method for the content of Peiminine in fritillaria thunbergii |
| CN112147243A (en) * | 2020-08-26 | 2020-12-29 | 浙江省人民医院 | Detection method for simultaneously determining multiple active ingredients in lung-clearing medicament |
| CN112147243B (en) * | 2020-08-26 | 2022-08-02 | 浙江省人民医院 | Detection method for simultaneously determining multiple active ingredients in lung-clearing medicament |
| CN115372501A (en) * | 2022-07-27 | 2022-11-22 | 广州科曼生物科技有限公司 | Thunberg fritillary bulb or Hubei fritillary bulb contrast extract and preparation method and application thereof |
| CN115372501B (en) * | 2022-07-27 | 2024-03-26 | 广州科曼生物科技有限公司 | Control extract of fritillaria thunbergii or fritillaria hubei, preparation method and application thereof |
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Application publication date: 20160622 |