CN105929036A - Method for extracting nuciferine from lotus leaves - Google Patents
Method for extracting nuciferine from lotus leaves Download PDFInfo
- Publication number
- CN105929036A CN105929036A CN201610234682.1A CN201610234682A CN105929036A CN 105929036 A CN105929036 A CN 105929036A CN 201610234682 A CN201610234682 A CN 201610234682A CN 105929036 A CN105929036 A CN 105929036A
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- China
- Prior art keywords
- extraction
- extracting
- nuciferine
- folium nelumbinis
- static
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses a method for extracting nuciferine from lotus leaves. The method comprises the following steps: step one, grinding lotus leaves, and sieving; step two, weighing 0.5 part by weight of grosvenor momordica fruit powder and 0.5 part by weight of diatomite, evenly mixing, and saving the mixture for later use; step three, transferring the mixture obtained in the step two into an extraction tank provided with a filter membrane, adding a proper amount of diatomite until the diatomite reaches the opening of the extraction tank; covering extraction tank by a cover to carry out static extraction; and after extraction, obtaining a liquid extract; wherein the extraction conditions are as follows: the extracting solvent is methanol, the extraction temperature is 90 DEG C, the static extraction lasts for 5 minutes, the flush volume is 100%, and static circulation is performed for two times. The provided method has the advantages of simple operation, high precision of separation and purification, short time, and little using amount of sample.
Description
Technical field
The present invention relates to test in laboratory field, a kind of method extracting nuciferine from Folium Nelumbinis.
Background technology
Pharmacopeia in 2015 have recorded the extracting method of the nuciferine in Folium Nelumbinis: takes this product coarse powder about 0.5g, accurately weighed, puts tool plug
In conical flask, accurate addition methanol 50ml, weighed weight, it is heated to reflux 2.5 hours, lets cool, more weighed weight, use methanol
Supplying the weight of less loss, shake up, filter, precision measures subsequent filtrate 5ml, puts in 10ml measuring bottle, adds water to scale, shakes up,
Obtain.
Liquid chromatographic detection condition is: with octadecylsilane chemically bonded silica as filler；With acetonitrile one water one triethylamine glacial acetic acid
(27:70.6:1.6:0.78) for flowing phase；Detection wavelength is 270nm.Number of theoretical plate is calculated should be not less than by nuciferine peak
2000。
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 a kind of method extracting nuciferine from Folium Nelumbinis, the method is simple to operate, the essence of separating-purifying
Degree height, the used time is short, and amount of samples is few.
The technical scheme that the present invention provides is: a kind of method extracting nuciferine from Folium Nelumbinis, comprises the following steps:
Step 1: after Folium Nelumbinis is pulverized, sieve；
Step 2: weigh 0.5 weight portion mangosteen powder, mixs homogeneously stand-by with 0.5 weight portion kieselguhr；
Step 3: the mixture in step 2 is moved in the abstraction pool putting filter membrane in advance well, add appropriate kieselguhr to reaching
Chi Kou to abstraction pool；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is methanol；Extraction temperature 90 DEG C；Static extracting time 5min；Flush volume 100%；
Quiet cycle number of times 2 times.
In the above-mentioned method extracting nuciferine from Folium Nelumbinis, the volume of described abstraction pool is 10ml.
In the above-mentioned method extracting nuciferine from Folium Nelumbinis, the pressure of described static extracting is 1500psi.
In the above-mentioned method extracting nuciferine from Folium Nelumbinis, the purge time of described static extracting is 60s.
In the above-mentioned method extracting nuciferine from Folium Nelumbinis, described step 3 also includes step 4 after terminating, itself particularly as follows:
By being centrifuged 5min after extract methanol dilution under 15000r/min, take supernatant.
In the above-mentioned method extracting nuciferine from Folium Nelumbinis, the instrument that described ASE extraction is used is that ASE350 is fast
Quick-dissolving agent abstraction instrument.
The present invention is after using technique scheme, and it has the beneficial effect that
The detection method of the present invention is simple to operate, and effect of extracting is consistent with the precision of official method, and reproducible, amount of samples is few,
Extraction time is short.
Accompanying drawing explanation
Fig. 1 is the rectangular plots of the chromatography nuciferine validation verification of the present invention；
Fig. 2 is the chromatogram of the present invention.
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 the present invention
Any restriction.
Embodiment 1:
Size-reduced for Folium Nelumbinis machine is pulverized, excessively No. three sieves, about 0.5g, accurately weighed, mix homogeneously with 0.5g kieselguhr, stand-by,
It is moved into and puts filter membrane in advance wellAdding proper amount of silicon diatomaceous earth in 10ml abstraction pool, shaking is allowed to Chi Kou same gently
On one horizontal line, tighten abstraction pool upper cover.After extraction terminates, extract is shifted in 25ml volumetric flask, with methanol dilution extremely
Scale, under 15000r/min, centrifugal 5min, takes supernatant, enters LC and measures.
Extraction conditions (being shown in Table 1) is:
Table 1
Analysis method is LC liquid chromatography, liquid-phase chromatographic analysis condition:
A) the double ternary liquid phase (U-3000) of instrument: Thermo
B) chromatographic column Eclipse XDB (C185 μm 4.6 × 150mm, i.e. carbon 18 chromatographic column, diameter 4.6mm, length 150mm,
Particle diameter 5 μm)
C) column temperature: 40 DEG C
D) flow velocity: 0.5mL/min
E) flowing phase: acetonitrile-water-triethylamine-glacial acetic acid (volume ratio 27:70.6:1.6:0.78)
F) detection wavelength: 270nm
Chromatography validation verification:
Take nuciferine reference substance appropriate, accurately weighed, add methanol and make every 1ml solution containing 16 μ g, to obtain final product.
Take nuciferine reference substance solution (concentration: 0.1587mg/ml), respectively precision draw this solution 1 μ l, 2 μ l, 4 μ l, 5
μ l, 10 μ l enter LC and measure, and measure according to said method, the results detailed in Table 2.With absolute sample size (μ g)-average
Peak area carries out linear regression, tries to achieve regression equation: y=5.7934x-0.0315, R2=0.9997.Nuciferine is 0.1587～0.9122
In good linear relationship in μ g range, the rectangular plots of this linear relationship is shown in Fig. 1.Using of nuciferine reference substance is above-mentioned
The chromatogram that liquid chromatography analysis obtains, refers to the collection of illustrative plates being numbered corresponding to S-1 in Fig. 2.
Table 2 nuciferine linear relationship
The repeatability checking of the extracting process of embodiment 1:
Take sample (lot number: the 150820) 0.5g of identical lot number, totally 6 parts, accurately weighed, extract by ASE extracting method
Need testing solution, sample size is 8 μ l, with above-mentioned chromatographic condition parallel test, records the content of nuciferine in sample and is shown in Table 2,
RSD is 3.5%, and test shows that ASE extracting method repeatability is good, the results detailed in Table 3.
Table 3
The degree of accuracy test of the extracting process of embodiment 1
Using the ASE extracting process of embodiment 1 and the extracting process of pharmacopeia to extract Folium Nelumbinis, Folium Nelumbinis is 4 batches, and lot number divides
It is not 1512008,20150501,150820,1508144；
The ASE extracting process of embodiment 1 uses the machine that same model specification is the most different to carry out parallel to a batch of Folium Nelumbinis
Testing twice, respectively ASE1 and ASE2 represents.
In Fig. 2, the collection of illustrative plates corresponding to label 114-2-1 is the chromatogram that sample 1508144 obtains according to the method described in pharmacopeia；
Being numbered the collection of illustrative plates corresponding to orthogonal 8-1 in Fig. 2 is that sample 1508144 obtains according to the method described in embodiment 1
Chromatogram.
Concrete test result see table 4；
Table 4
Above-described be only presently preferred embodiments of the present invention, all made in the range of the spirit and principles in the present invention any amendment,
Equivalent and improvement etc., should be included within the scope of the present invention.
Claims (6)
1. the method extracting nuciferine from Folium Nelumbinis, it is characterised in that comprise the following steps:
Step 1: after Folium Nelumbinis is pulverized, sieve；
Step 2: weigh 0.5 weight portion mangosteen powder, mixs homogeneously stand-by with 0.5 weight portion kieselguhr；
Step 3: the mixture in step 2 is moved in the abstraction pool putting filter membrane in advance well, add appropriate kieselguhr to reaching
Chi Kou to abstraction pool；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is methanol；Extraction temperature 90 DEG C；Static extracting time 5min；Flush volume 100%；
Quiet cycle number of times 2 times.
The method extracting nuciferine from Folium Nelumbinis the most according to claim 1, it is characterised in that the body of described abstraction pool
Amass as 10ml.
The method extracting nuciferine from Folium Nelumbinis the most according to claim 1, it is characterised in that described static extracting
Pressure is 1500psi.
The method extracting nuciferine from Folium Nelumbinis the most according to claim 1, it is characterised in that described static extracting
Purge time is 60s.
The method extracting nuciferine from Folium Nelumbinis the most according to claim 1, it is characterised in that described step 3 terminates
After also include step 4, itself particularly as follows: by after extract methanol dilution under 15000r/min centrifugal 5min, take supernatant.
The method extracting nuciferine from Folium Nelumbinis the most according to claim 1, it is characterised in that described ASE extraction
The instrument that method is used is ASE350 Accelerate solvent extraction instrument.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610234682.1A CN105929036A (en) | 2016-04-15 | 2016-04-15 | Method for extracting nuciferine from lotus leaves |
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| CN201610234682.1A CN105929036A (en) | 2016-04-15 | 2016-04-15 | Method for extracting nuciferine from lotus leaves |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106924991A (en) * | 2017-04-17 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method of recinine in ASE methods extraction castor bean |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102258578A (en) * | 2010-05-25 | 2011-11-30 | 天津中医药大学 | Novel lotus leaf total alkaloid extract and preparation method as well as application thereof |
| CN103494178A (en) * | 2013-09-30 | 2014-01-08 | 浙江工业大学 | Method for extracting lentinus edodes total alkaloid |
| CN103830374A (en) * | 2014-03-06 | 2014-06-04 | 天津中医药大学 | Application of three-leaf glycolipid-removal medicine in hyperuricemia |
| WO2015152577A3 (en) * | 2014-04-02 | 2015-11-26 | 연세대학교 산학협력단 | Composition for preventing and treating bone disease |
-
2016
- 2016-04-15 CN CN201610234682.1A patent/CN105929036A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102258578A (en) * | 2010-05-25 | 2011-11-30 | 天津中医药大学 | Novel lotus leaf total alkaloid extract and preparation method as well as application thereof |
| CN103494178A (en) * | 2013-09-30 | 2014-01-08 | 浙江工业大学 | Method for extracting lentinus edodes total alkaloid |
| CN103830374A (en) * | 2014-03-06 | 2014-06-04 | 天津中医药大学 | Application of three-leaf glycolipid-removal medicine in hyperuricemia |
| WO2015152577A3 (en) * | 2014-04-02 | 2015-11-26 | 연세대학교 산학협력단 | Composition for preventing and treating bone disease |
Non-Patent Citations (4)
| Title |
|---|
| FENG LIU 等: "Cloud Point Extraction and Pre-Concentration of Four Alkaloids in Nelumbo nucifera Leaves by Ultrahigh Pressure-Assisted Extraction", 《SEPARATION SCIENCE AND TECHNOLOGY》 * |
| 徐榕青: "《福建道地药材现代研究》", 31 October 2014, 福州：福建科学技术出版社 * |
| 李攻科 等: "《样品前处理仪器与装置》", 31 May 2007, 北京：化学工业出版社 * |
| 李文龙 等: "加速溶剂萃取-高效液相色谱-电喷雾飞行时间质谱联用分析莲子心中生物碱", 《分析化学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106924991A (en) * | 2017-04-17 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method of recinine in ASE methods extraction castor bean |
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Application publication date: 20160907 |