CN105717241A - Determination method of chlorogenic acid in wild chrysanthemum flower - Google Patents
Determination method of chlorogenic acid in wild chrysanthemum flower Download PDFInfo
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- CN105717241A CN105717241A CN201610268356.2A CN201610268356A CN105717241A CN 105717241 A CN105717241 A CN 105717241A CN 201610268356 A CN201610268356 A CN 201610268356A CN 105717241 A CN105717241 A CN 105717241A
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- extraction
- flos chrysanthemi
- chrysanthemi indici
- assay method
- chlorogenic acid
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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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- 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
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- General Health & Medical Sciences (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention discloses a determination method of chlorogenic acid in wild chrysanthemum flower. The determination method comprises the following steps: (1) grinding and sieving the wild chrysanthemum flower, mixing 0.25 part of wild chrysanthemum flower with 0.3g of diatomite, adding the mixture into an extraction pond which is pre-paved with a filter membrane, and carrying out static extraction to obtain extraction liquid, wherein the extraction conditions are as follows: an extracting solvent is a mixture of ethanediamine and ethanol in a weight ratio of 0.1 to 9.9, the extraction temperature is 100 DEG C, the static extraction time is 5 minutes, the flushing volume is 100%, the static cycle index is 1, and the extraction pressure is 1500psi; (2) carrying out dilution and centrifuging on extract liquid, so as to obtain supernate; and (3) analyzing the supernate by virtue of a liquid chromatography. Compared with extraction of reflux extraction method and detection of a high performance liquid chromatography, the determination method has the advantage that the result is relatively accurate.
Description
Technical field
The present invention relates to test in laboratory field, particularly the assay method of the chlorogenic acid in a kind of Flos Chrysanthemi Indici.
Background technology
HeraldofmedicineVOL28No8Augest2009 discloses the content of Flos Chrysanthemi Indici by HPLC Content of Chlorogenic Acid, it adopts the method extraction of reflux, extract, to obtain chlorogenic acid, then pass through high performance liquid chromatography measurement, its measurement time longer and extract certainty of measurement have much room for improvement.
Along with the development of Fast Detection Technique, can obtaining the plurality of active ingredients in Chinese medicine by ultrasonic extraction method, Accelerate solvent extraction method, difficult point is in that, how effectively to adjust the purpose that each parameter reaches each component is accurately tested.
Summary of the invention
It is an object of the invention to provide the assay method of chlorogenic acid in a kind of Flos Chrysanthemi Indici, the method is extracted compared to reflux extraction and carries out high performance liquid chromatography detection to obtain result more accurate.
Technical scheme provided by the invention is: the assay method of the chlorogenic acid in a kind of Flos Chrysanthemi Indici, comprises the following steps:
Step 1: by Flos Chrysanthemi Indici grinding and sieving, the Herba Dendranthematis indici pollen taking 0.25 weight portion mixes with 0.3g kieselguhr, join and be equipped with in the abstraction pool of filter membrane in advance and carry out static extracting obtain extract, extraction conditions is: extractant is weight ratio is the mixture of the ethylenediamine of 0.1:9.9 and ethanol, extraction temperature 100 DEG C, the static extracting time is 5min, flush volume 100%, quiet cycle number of times is 1 time, extracting pressure 1500psi；
Step 2: after centrifugal for extract dilution, obtain supernatant；
Step 3: adopt liquid chromatography to be analyzed supernatant；
Wherein, the analysis condition of liquid chromatography is:
A) instrument: chromatograph of liquid
B) chromatographic column C183μm3×100mm
C) column temperature: 40 DEG C
D) flow velocity: 0.5mL/min
E) mobile phase: acetonitrile-water, volume ratio is 4:6
F) detection wavelength: 326nm.
In the assay method of the chlorogenic acid in above-mentioned Flos Chrysanthemi Indici, the volume of described abstraction pool is 5ml, and the purge time of described static extracting is 60s.
In the assay method of the chlorogenic acid in above-mentioned Flos Chrysanthemi Indici, step 2 particularly as follows: by after the mixture dilution of ethylenediamine that extract weight ratio is 0.1:9.9 and ethanol under 15000r/min centrifugal 5min, take supernatant.
In the assay method of the chlorogenic acid in above-mentioned Flos Chrysanthemi Indici, the instrument used by liquid-phase chromatographic analysis is: the double; two ternary liquid phase chromatograph of ThermoU-3000, chromatographic column is ThermoSyncronisC18 chromatographic column.
In the assay method of the chlorogenic acid in above-mentioned Flos Chrysanthemi Indici, extracting used instrument in described step 1 is ASE350 Accelerate solvent extraction instrument
The present invention is after adopting technique scheme, and it has the beneficial effect that
Chlorogenic acid row in Flos Chrysanthemi Indici is extracted by the present invention by ASE static state fast solutions extracting process, and adjusts liquid chromatography parameter, reaches the purpose to the more fast and convenient and high-precision mensuration chlorogenic acid in Flos Chrysanthemi Indici of the chlorogenic acid in Flos Chrysanthemi Indici.
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:
The assay method of the chlorogenic acid in a kind of Flos Chrysanthemi Indici: size-reduced for Flos Chrysanthemi Indici machine is pulverized, excessively No. three sieves, about 0.25g, 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 5ml 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, be diluted to scale with the mixture of the ethylenediamine that weight ratio is 0.1:9.9 and ethanol, under 15000r/min, centrifugal 5min, 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 μm of 3 × 100mm, i.e. carbon 18 chromatographic column, diameter 3mm, length 100mm, particle diameter 3 μm)
C) column temperature: 40 DEG C
D) flow velocity: 0.5mL/min
E) mobile phase: acetonitrile-water, the volume ratio under 20 DEG C of conditions is 4:6
F) detection wavelength: 326nm
The Flos Chrysanthemi Indici taking 3 lot numbers is tested, lot number respectively 1510020,151001,20150701, adopting the extraction of embodiment 1 and detection method to test, reflux, extract, and the high performance liquid chromatography the product of identical lot number recorded according to background technology are tested simultaneously.The test result of the chlorogenic acid in Flos Chrysanthemi Indici such as table 1 below:
Table 1
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 (5)
1. the assay method of the chlorogenic acid in a Flos Chrysanthemi Indici, it is characterised in that comprise the following steps:
Step 1: by Flos Chrysanthemi Indici grinding and sieving, the Herba Dendranthematis indici pollen taking 0.25 weight portion mixes with 0.3g kieselguhr, join and be equipped with in the abstraction pool of filter membrane in advance and carry out static extracting obtain extract, extraction conditions is: extractant is weight ratio is the mixture of the ethylenediamine of 0.1:9.9 and ethanol, extraction temperature 100 DEG C, the static extracting time is 5min, flush volume 100%, quiet cycle number of times is 1 time, extracting pressure 1500psi；
Step 2: after centrifugal for extract dilution, obtain supernatant；
Step 3: adopt liquid chromatography to be analyzed supernatant；
Wherein, the analysis condition of liquid chromatography is:
A) instrument: chromatograph of liquid
B) chromatographic column C183μm3×100mm
C) column temperature: 40 DEG C
D) flow velocity: 0.5mL/min
E) mobile phase: acetonitrile-water, volume ratio is 4:6
F) detection wavelength: 326nm.
2. the assay method of the chlorogenic acid in Flos Chrysanthemi Indici according to claim 1, it is characterised in that the volume of described abstraction pool is 5ml, the purge time of described static extracting is 60s.
3. the assay method of the total flavones in Flos Chrysanthemi Indici according to claim 1, it is characterised in that step 2 particularly as follows: by after the mixture dilution of ethylenediamine that extract weight ratio is 0.1:9.9 and ethanol under 15000r/min centrifugal 5min, take supernatant.
4. the double; two ternary liquid phase chromatograph of the assay method of the total flavones in Flos Chrysanthemi Indici according to claim 1, it is characterised in that the instrument used by liquid-phase chromatographic analysis is: ThermoU-3000, chromatographic column is ThermoSyncronisC18 chromatographic column.
5. the assay method of the total flavones in Flos Chrysanthemi Indici according to claim 1, it is characterised in that extracting used instrument in described step 1 is ASE350 Accelerate solvent extraction instrument.
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| CN201610268356.2A CN105717241A (en) | 2016-04-27 | 2016-04-27 | Determination method of chlorogenic acid in wild chrysanthemum flower |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106841478A (en) * | 2017-04-20 | 2017-06-13 | 广西壮族自治区梧州食品药品检验所 | It is a kind of at the same determine chrysanthemum indicum in seven kinds of methods of the content of composition |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101034085A (en) * | 2007-01-17 | 2007-09-12 | 广州星群（药业）股份有限公司 | Establishment of Xiasangju preparations fingerprint pattern and fingerprint pattern thereof |
| CN102253135A (en) * | 2011-04-19 | 2011-11-23 | 中国广州分析测试中心 | Method for establishing fingerprint of Deng's herbal tea granules and standard fingerprint thereof |
| CN102928523A (en) * | 2011-08-11 | 2013-02-13 | 上海雷允上科技发展有限公司 | Wild chrysanthemum flower fingerprint determination method, its application, and wild chrysanthemum flower quality detection method |
-
2016
- 2016-04-27 CN CN201610268356.2A patent/CN105717241A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101034085A (en) * | 2007-01-17 | 2007-09-12 | 广州星群（药业）股份有限公司 | Establishment of Xiasangju preparations fingerprint pattern and fingerprint pattern thereof |
| CN102253135A (en) * | 2011-04-19 | 2011-11-23 | 中国广州分析测试中心 | Method for establishing fingerprint of Deng's herbal tea granules and standard fingerprint thereof |
| CN102928523A (en) * | 2011-08-11 | 2013-02-13 | 上海雷允上科技发展有限公司 | Wild chrysanthemum flower fingerprint determination method, its application, and wild chrysanthemum flower quality detection method |
Non-Patent Citations (2)
| Title |
|---|
| 罗进 等: "五种菊花中绿原酸含量的检测和比较", 《绵阳师范学院学报》 * |
| 金诚 等: "用加速溶剂萃取及制备型高效液相色谱法从烟梗中制取多酚对照品", 《理化检验-化学分册》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106841478A (en) * | 2017-04-20 | 2017-06-13 | 广西壮族自治区梧州食品药品检验所 | It is a kind of at the same determine chrysanthemum indicum in seven kinds of methods of the content of composition |
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Application publication date: 20160629 |