CN105954390A - Method for detecting content of kaempferide in momordica grosvenori tea by using ASE-HPLC - Google Patents
Method for detecting content of kaempferide in momordica grosvenori tea by using ASE-HPLC Download PDFInfo
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- CN105954390A CN105954390A CN201610259369.3A CN201610259369A CN105954390A CN 105954390 A CN105954390 A CN 105954390A CN 201610259369 A CN201610259369 A CN 201610259369A CN 105954390 A CN105954390 A CN 105954390A
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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
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention provides a method for detecting content of kaempferide in momordica grosvenori tea by using ASE-HPLC, and aims at providing the method which has a high analysis efficiency and good repeatability of detection result for detecting content of kaempferide in momordica grosvenori tea by using ASE-HPLC. The method includes taking the sample, weighing the sample accurately, porphyrizing the sample, putting 1g of the sample into 10ml extraction pool, performing extraction for the sample by using 70% ethanol, using methanol as an extraction solvent to perform extraction, drying the extract by vacuum distillation, adding 14ml methanol into the residue to dissolve the residue, adding 10% phosphoric acid solution 5ml, performing heating reflux in water bath for 30min, cooling the product, quantificationally transferring the product into a 25ml volumetric flask, diluting the product to the scale with methanol, sucking 1.5ml solution into a 2ml centrifuge tube having 300mg PSA, swirling the solution for 2min, centrifuging the solution for 3min at 15000r/min, and taking supernatant to perform high performance liquid chromatography analysis. The invention belongs to the technical field of chemical detection.
Description
Technical field
The present invention provides a kind of method measuring kaempferide content, specifically, is a kind of
ASE-HPLC measures the method for kaempferide content in " Luohan " fruit tea；Belong to chemical detection technique
Field.
Background technology
" Luohan " fruit tea is the medicinal tea being extracted by Fructus Momordicae, being processed into.Through substantial amounts of clinical examination
Verifying bright, " Luohan " fruit tea is cough caused for treatment acute bronchitis phlegm-heat obstructing in the lung, expectorant
The diseases such as many, xerostomia have good result, and root according to the literature, removes containing calabash alkanes in Fructus Momordicae
Outside compound, 2 kind flavonoid glycosides are also obtained；Owing to flavone compound has antiinflammatory, strong
The heart, blood pressure lowering, coronary artery dilator, reduction cholesterol, diuresis, eliminating phlegm and stopping cough, protect the liver
Effect, therefore by measuring the content of flavone compound in " Luohan " fruit tea, reach to control product
The purpose of quality, quercetin content in Fructus Momordicae fresh fruit is studied by forefathers.
Summary of the invention
For above-mentioned deficiency, it is an object of the invention to provide a kind of analysis efficiency high, detection knot
The ASE-HPLC that fruit has reappeared measures the method for kaempferide content in " Luohan " fruit tea.
For solving above-mentioned technical problem, the technical scheme that the present invention provides is as follows:
A kind of ASE-HPLC measures the method for kaempferide content in " Luohan " fruit tea, includes successively
Following step:
1) this product is taken, accurately weighed, finely ground, take 1g and be placed in 10mL abstraction pool, use
Sample is extracted by 70% ethanol, and described Extracting temperature is 60 DEG C, static extraction time
For 5min, extraction time is 1 time, flush volume 65%, then with methanol as Extraction solvent,
Extracting temperature is 70 DEG C, and static extraction time is 3min, and extraction time is 2 times；Decompression is steamed
Dry, residue adds methanol 14ml makes dissolving, adds 10% phosphoric acid solution 5ml, puts heating in water bath and return
Flow 30 minutes, let cool, be quantitatively transferred in 25ml measuring bottle, with methanol dilution to scale,
Draw 1.5mL in equipped with in the 2mL centrifuge tube of 300mg PSA, whirlpool 2min,
15000r/min is centrifuged 3min, takes supernatant and carries out high-efficient liquid phase analysis；
2) when high performance liquid chromatography is analyzed, parameter is provided that
Flowing phase: 70% alcohol-water-acetonitrile, reconciling pH value with formic acid is 4.0；Flow velocity:
1ml/min；Column temperature: 35 DEG C；
Chromatographic column: Phenomenex C18 post；
Detection wavelength 271nm；
In described flowing mutually the volume ratio of 70% alcohol-water-acetonitrile be 10:10:80～
25:25:50；Described flowing is 70% alcohol-water-second in 0 minute to 4 minutes sections
The volume ratio of nitrile is that 30:30:40 rises to 35:35:30；Then at 4 minutes to 9 minutes
In section, the volume ratio of 70% alcohol-water-acetonitrile is constant at 40:40:20, then in 9-12 minute
The volume ratio of 70% alcohol-water-acetonitrile is constant at 20:20:60.
Further, above-mentioned a kind of ASE-HPLC measures kaempferide content in " Luohan " fruit tea
Method, the specification of described chromatographic column is 5 μm, 4.6mm × 250mm.
Compared with prior art, the technical scheme that the present invention provides measures Rhizoma Kaempferiae by HPLC method
Cellulose content, reflects the content of flavone compound, and cubage method has been carried out reality
Test discussion research.By ASE rapid extraction, gradient elution detects, and this operational approach is simple
Quickly, result shows that this law is accurate, reliably, noiseless, and favorable reproducibility can be used for arhat
The quality control of fruit juice.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the claim of the present invention is done the most in detail
Illustrate, but do not constitute any limitation of the invention, any in the claims in the present invention protection
The amendment of the limited number of time that scope is made, still within the claims of the present invention.
Involved in the present invention to percentage composition concentration, in addition to specified otherwise, solute is liquid
Be volumetric concentration, solute be solid be mass concentration.
Embodiment 1
A kind of ASE-HPLC measures the method for kaempferide content in " Luohan " fruit tea, includes successively
Following step:
Take this product, accurately weighed, finely ground, take 1g and be placed in 10mL abstraction pool, with 70%
Sample is extracted by ethanol, and described Extracting temperature is 60 DEG C, and static extraction time is
5min, extraction time is 1 time, flush volume 65%, then with methanol as Extraction solvent, carries
Taking temperature is 70 DEG C, and static extraction time is 3min, and extraction time is 2 times；Decompression is steamed
Dry, residue adds methanol 14ml makes dissolving, adds 10% phosphoric acid solution 5ml, puts heating in water bath and return
Flow 30 minutes, let cool, be quantitatively transferred in 25ml measuring bottle, with methanol dilution to scale,
Draw 1.5mL in equipped with in the 2mL centrifuge tube of 300mg PSA, whirlpool 2min,
15000r/min is centrifuged 3min, takes supernatant and carries out high-efficient liquid phase analysis；
2) when high performance liquid chromatography is analyzed, parameter is provided that
Flowing phase: 70% alcohol-water-acetonitrile, reconciling pH value with formic acid is 4.0；Flow velocity:
1ml/min；Column temperature: 35 DEG C；
Chromatographic column: Phenomenex C18 post (5 μm, 4.6mm × 250mm)；
Detection wavelength 271nm；
In described flowing mutually the volume ratio of 70% alcohol-water-acetonitrile be 10:10:80～
25:25:50；Described flowing is 70% alcohol-water-second in 0 minute to 4 minutes sections
The volume ratio of nitrile is that 30:30:40 rises to 35:35:30；Then at 4 minutes to 9 minutes
In section, the volume ratio of 70% alcohol-water-acetonitrile is constant at 40:40:20, then in 9-12 minute
The volume ratio of 70% alcohol-water-acetonitrile is constant at 20:20:60.
Phosphorus pentoxide drying under reduced pressure kaempferide reference substance overnight of learning from else's experience is appropriate, accurate title
Fixed, add methanol and make every 1ml solution containing 10 μ g, obtain reference substance solution.
Draw reference substance solution 10 μ l, need testing solution and negative sample solution each 20 respectively
μ l, injects high performance liquid chromatograph, by above-mentioned chromatographic condition record chromatogram, kaempferide peak
Mensuration noiseless, the retention time of kaempferide is about 12 minutes, and kaempferide peak is with adjacent
Near honeybee separating degree is good.
Claims (2)
1. a method for kaempferide content during ASE-HPLC measures " Luohan " fruit tea, it is special
Levy and be, comprise the steps: successively
1) this product is taken, accurately weighed, finely ground, take 1g and be placed in 10mL abstraction pool, use
Sample is extracted by 70% ethanol, and described Extracting temperature is 60 DEG C, static extraction time
For 5min, extraction time is 1 time, flush volume 65%, then with methanol as Extraction solvent,
Extracting temperature is 70 DEG C, and static extraction time is 3min, and extraction time is 2 times；Decompression is steamed
Dry, residue adds methanol 14ml makes dissolving, adds 10% phosphoric acid solution 5ml, puts heating in water bath and return
Flow 30 minutes, let cool, be quantitatively transferred in 25ml measuring bottle, with methanol dilution to scale,
Draw 1.5mL in equipped with in the 2mL centrifuge tube of 300mg PSA, whirlpool 2min,
15000r/min is centrifuged 3min, takes supernatant and carries out high-efficient liquid phase analysis；
2) when high performance liquid chromatography is analyzed, parameter is provided that
Flowing phase: 70% alcohol-water-acetonitrile, reconciling pH value with formic acid is 4.0；Flow velocity:
1ml/min；Column temperature: 35 DEG C；
Chromatographic column: Phenomenex C18 post；
Detection wavelength 271nm；
In described flowing mutually the volume ratio of 70% alcohol-water-acetonitrile be 10:10:80～
25:25:50；Described flowing is 70% alcohol-water-second in 0 minute to 4 minutes sections
The volume ratio of nitrile is that 30:30:40 rises to 35:35:30；Then at 4 minutes to 9 minutes
In section, the volume ratio of 70% alcohol-water-acetonitrile is constant at 40:40:20, then in 9-12 minute
The volume ratio of 70% alcohol-water-acetonitrile is constant at 20:20:60.
A kind of ASE-HPLC the most according to claim 1 measures mountain in " Luohan " fruit tea
How the method for cellulose content, it is characterised in that the specification of described chromatographic column is 5 μm, 4.6
mm×250mm。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610259369.3A CN105954390A (en) | 2016-04-25 | 2016-04-25 | Method for detecting content of kaempferide in momordica grosvenori tea by using ASE-HPLC |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101156893A (en) * | 2005-02-07 | 2008-04-09 | 贵阳云岩西创药物科技开发有限公司 | Mass control method of apricot red injection |
| CN105203673A (en) * | 2015-11-13 | 2015-12-30 | 广西医科大学制药厂 | High performance liquid chromatography detection method of compound nightshade inflammation-diminishing tablets |
-
2016
- 2016-04-25 CN CN201610259369.3A patent/CN105954390A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101156893A (en) * | 2005-02-07 | 2008-04-09 | 贵阳云岩西创药物科技开发有限公司 | Mass control method of apricot red injection |
| CN105203673A (en) * | 2015-11-13 | 2015-12-30 | 广西医科大学制药厂 | High performance liquid chromatography detection method of compound nightshade inflammation-diminishing tablets |
Non-Patent Citations (2)
| Title |
|---|
| 刘丽芳: "《中药分析实验与指导》", 30 September 2015 * |
| 金丽鑫: "金钱草对照药材标定技术标准的研究", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
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