CN102253145B - Method for detecting 5,7-dyhydroxy chromone, eriodictyol and luteolin in peanut shell simultaneously - Google Patents
Method for detecting 5,7-dyhydroxy chromone, eriodictyol and luteolin in peanut shell simultaneously Download PDFInfo
- Publication number
- CN102253145B CN102253145B CN 201110194346 CN201110194346A CN102253145B CN 102253145 B CN102253145 B CN 102253145B CN 201110194346 CN201110194346 CN 201110194346 CN 201110194346 A CN201110194346 A CN 201110194346A CN 102253145 B CN102253145 B CN 102253145B
- Authority
- CN
- China
- Prior art keywords
- eriodictyol
- mobile phase
- peanut shell
- cyanidenon
- chromone
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention belongs to the field of food detection, and particularly relates to a method for detecting 5,7-dyhydroxy chromone, eriodictyol and luteolin which serve as main active ingredients in a peanut shell simultaneously. In the method, three active ingredients are detected by high performance liquid chromatography and by using octadecyl silane bonded silica gel as a filling agent and methanol and an aqueous gradient elution solvent as a mobile phase and regulating the pH value by acid; and sample introduction is performed once, and a chromatographic peak of each component is better separated to obtain the detection effect with high accuracy and repeatability. The method for detecting the 5,7-dyhydroxy chromone, the eriodictyol and the luteolin in the peanut shell is simple, easy and convenient to operate, low in cost and high in efficiency, and is a shortcut for the quality control of the raw materials and products.
Description
Technical field
The invention belongs to the food inspection field, be specifically related to a kind ofly can detect simultaneously in the peanut shell 5, the method for 7-dihydroxy chromone, eriodictyol and cyanidenon.
Background technology
Peanut (Peanut) derives from the dry pod of pulse family annual herb plant peanut (Arachis hypogaea L.), and peanut shell (Peanut hull) is the shell of its pod.China's peanut shell aboundresources, cheap, have broad application prospects in medicine, industry, agricultural, field of health care food.Peanut shell among the people be Chinese herbal medicine, can treat that asthma, phlegm are many, hypertension etc.That flavones ingredient take cyanidenon as representative in the peanut shell has is hypotensive, reducing blood lipid, coronary artery dilator, anti-oxidant, antibechic, eliminating phlegm and relieving asthma, antimicrobial antiphlogistic, enhancing immunity and the multiple pharmacologically active such as antitumor.Studies show that, flavone compound and its physiologically active contained in the peanut shell are closely related.
5,7-dihydroxy chromone, eriodictyol and cyanidenon are the major function compositions in the peanut shell, only have in the bibliographical information and measure in the peanut shell 5,7-dihydroxy chromone and eriodictyol and the method for measuring separately cyanidenon, and adopting high performance liquid chromatography to detect simultaneously 5, the method for 7-dihydroxy chromone, eriodictyol and cyanidenon there is not yet report.
Summary of the invention
For solving above-mentioned technical matters, the present invention is that a kind of method is simple, accuracy is high, favorable reproducibility can detect simultaneously 5, the method of 7-dihydroxy chromone, eriodictyol and cyanidenon, and can be used as the assay method of discriminating, content and the related substance of these three kinds of compositions.
Of the present inventionly a kind ofly can detect simultaneously in the peanut shell 5, the method for 7-dihydroxy chromone, eriodictyol and cyanidenon comprises following step:
(1) preparation of contrast solution: take by weighing respectively 5,7-dihydroxy chromone, eriodictyol and three kinds of reference substances of cyanidenon and add methyl alcohol dissolving, in contrast solution for standby;
(2) preparation of sample solution: be that 40～80 orders get sample powder with peanut shell impurity elimination, cleaning, crushed after being dried to its fineness, the sample thief powder, add the ultrasonic extraction of entry or organic solvent, the volume of described water or organic solvent and sample powder weight ratio are 10～40:1, centrifugal after extracting, supernatant is with the organic membrane filter of 0.45 μ m, and filtrate is testing sample solution;
(3) measure: respectively contrast solution and testing sample solution are injected high performance liquid chromatograph, be filling agent with octadecylsilane chemically bonded silica, carry out gradient elution, volumetric flow rate 1.0mL/min take methyl alcohol-aqueous acid as mobile phase, 30 ℃～40 ℃ of column temperatures detect wavelength 254～360nm;
(4) with variable concentrations contrast solution sample introduction drawing standard curve respectively, according in the typical curve calculation sample solution 5, the content of 7-dihydroxy chromone, eriodictyol and three kinds of components of cyanidenon.
Above injection high performance liquid chromatograph detecting step, mobile phase A is 0.2%～0.4% aqueous acid, and Mobile phase B is methyl alcohol, and gradient elution detects wavelength 254～360nm.
The acid of regulating aqueous acid pH value in the mobile phase A is any in formic acid, acetic acid or the phosphoric acid.
Carry out gradient elution take methyl alcohol-aqueous acid as mobile phase, any in interpolation formic acid, acetic acid or the phosphoric acid is in ultrapure water, and mixing makes into 0.2%～0.4% aqueous acid.
Mobile phase is changed to the degree such as 0～3min, 5% Mobile phase B, 3～5min, 5%～30% Mobile phase B linear gradient, 5～30min, 30%～50% Mobile phase B linear gradient, 30～40min, 50%～60% Mobile phase B linear gradient in the gradient elution process of mobile phase.
Wherein the organic solvent described in the preparation process of sample solution is at least a in water, ethanol, methyl alcohol, the acetone.
The technical barrier that method of the present invention solves is, because in three kinds of compositions to be measured, 5, the optimum measurement wavelength of 7-dihydroxy chromone is 256 and 294nm, eriodictyol is 288nm, cyanidenon is 253 and 350nm, therefore under same wavelength, be difficult to detect simultaneously this three kinds of materials, the present invention has found an only wavelength sensing range and best detection wavelength, reach in wavelength coverage of the present invention under the given detection wavelength of the present invention, three kinds of materials of above this all can detect more accurately.
The present invention solves the another one technical matters, adopts isocratic elution to be difficult to the thorough wash-out of other impurity composition in these three kinds of compositions and the sample separately adopt gradient elution of the present invention, so that these three kinds of substances separate fast, and obtains Accurate Determining.
The most outstanding characteristics of the present invention are, select suitable detection wavelength, by the eluent gradient wash-out, can carry out effective separation to the component of complex sample by high performance liquid chromatography, once measure simultaneously content and the related substances of 5,7-dihydroxy chromone, eriodictyol and cyanidenon.
The invention has the beneficial effects as follows, can detect these three kinds of compositions of 5,7-dihydroxy chromone, eriodictyol and cyanidenon simultaneously fast and accurately, minute is no more than 40min, than independent respectively these three kinds of compositions are detected the time of having saved greatly, improved detection efficiency; And method precision of the present invention is high, good stability, and other compositions and auxiliary material do not affect mensuration in the sample, and the recovery of high, medium and low concentration is all better, favorable reproducibility, method is simple to operate, and is reliable and stable, practical, is fit to very much the control of product quality.
Description of drawings
Fig. 1 is the detection figure that the present invention detects the method for 5,7-dihydroxy chromone, eriodictyol and cyanidenon simultaneously.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is further described, so that those skilled in the art understand the present invention.
The preparation of contrast solution: take by weighing 5,7-dihydroxy chromone, eriodictyol and cyanidenon three kinds of each 2.4mg of reference substance, 2.4mg and 3.8mg in the 25ml volumetric flask, add the dissolving of 100% chromatogram methyl alcohol, be settled to scale mark, in contrast solution for standby;
The preparation of solution to be measured: after peanut shell impurity elimination, cleaning, the drying, pulverize with medicinal herb grinder, cross 60 mesh sieves, accurately take by weighing peanut shell powder 1.000g, add the ultrasonic extraction of 30mL methyl alcohol 40min, filter and with the chromatogram methanol constant volume to 50mL, filtrate is used the 0.45um organic membrane filter, is testing sample solution (being equivalent to peanut hull meal 20mg/mL);
Assay method: with variable concentrations reference substance solution, testing sample solution injection liquid chromatography, sample size 20 μ l; Mobile phase: 0.2% aqueous formic acid (A)-methyl alcohol (B), the degree such as 0-3min 5% Mobile phase B, 3～5min, 5%～30% Mobile phase B linear gradient, 5～30min, 30%～50% Mobile phase B linear gradient, 30～40min, 50%～60% Mobile phase B linear gradient, volumetric flow rate 1mL/min, 35 ℃ of column temperatures; Detect wavelength 294nm, retention time and the peak area of 5,7-dihydroxy chromone, eriodictyol and cyanidenon in the record 40min.
Data are processed: with variable concentrations reference substance sample introduction drawing standard curve respectively, according to typical curve with in the calculated by peak area test sample 5, the content of 7-dihydroxy chromone, eriodictyol and cyanidenon.
Claims (2)
1. one kind is detected in the peanut shell 5 simultaneously, and the method for 7-dihydroxy chromone, eriodictyol and cyanidenon comprises the steps:
The preparation of contrast solution: take by weighing 5,7-dihydroxy chromone, eriodictyol and cyanidenon three kinds of each 2.4mg of reference substance, 2.4mg and 3.8mg in the 25ml volumetric flask, add the dissolving of 100% chromatogram methyl alcohol, be settled to scale mark, in contrast solution for standby;
The preparation of solution to be measured: after peanut shell impurity elimination, cleaning, the drying, pulverize with medicinal herb grinder, cross 60 mesh sieves, accurately take by weighing peanut shell powder 1.000g, add ultrasonic extractions of 30mL methyl alcohol 40min, filtration and with the chromatogram methanol constant volume to 50mL, filtrate is used the 0.45um organic membrane filter, be testing sample solution, be equivalent to peanut hull meal 20mg/mL;
Assay method: with variable concentrations reference substance solution, testing sample solution injection liquid chromatography, sample size 20 μ l; Mobile phase: 0.2% aqueous formic acid (A)-methyl alcohol (B), 0-3min 5% Mobile phase B linear gradient, 3～5min, 5%～30% Mobile phase B linear gradient, 5～30min, 30%～50% Mobile phase B linear gradient, 30～40min, 50%～60% Mobile phase B linear gradient, volumetric flow rate 1mL/min, 35 ℃ of column temperatures; Detect wavelength 280-300nm, retention time and the peak area of 5,7-dihydroxy chromone, eriodictyol and cyanidenon in the record 40min;
Data are processed: with variable concentrations reference substance sample introduction drawing standard curve respectively, according to typical curve with in the calculated by peak area test sample 5, the content of 7-dihydroxy chromone, eriodictyol and cyanidenon.
2. detect simultaneously in the peanut shell 5 such as one kind of claim 1, the method for 7-dihydroxy chromone, eriodictyol and cyanidenon is characterized in that, detects wavelength 294nm in the described assay method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110194346 CN102253145B (en) | 2011-07-12 | 2011-07-12 | Method for detecting 5,7-dyhydroxy chromone, eriodictyol and luteolin in peanut shell simultaneously |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110194346 CN102253145B (en) | 2011-07-12 | 2011-07-12 | Method for detecting 5,7-dyhydroxy chromone, eriodictyol and luteolin in peanut shell simultaneously |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102253145A CN102253145A (en) | 2011-11-23 |
| CN102253145B true CN102253145B (en) | 2013-01-23 |
Family
ID=44980526
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110194346 Expired - Fee Related CN102253145B (en) | 2011-07-12 | 2011-07-12 | Method for detecting 5,7-dyhydroxy chromone, eriodictyol and luteolin in peanut shell simultaneously |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102253145B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101446573A (en) * | 2008-12-29 | 2009-06-03 | 甘肃奇正藏药有限公司 | Method for measuring content of luteolin in lamiophlomis rotata pharmaceutical preparation by liquid chromatography |
-
2011
- 2011-07-12 CN CN 201110194346 patent/CN102253145B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101446573A (en) * | 2008-12-29 | 2009-06-03 | 甘肃奇正藏药有限公司 | Method for measuring content of luteolin in lamiophlomis rotata pharmaceutical preparation by liquid chromatography |
Non-Patent Citations (8)
| Title |
|---|
| 不同产地花生壳中木犀草素的HPLC测定;唐丽萍等;《花生学报》;20051231;第34卷(第02期);1--4 * |
| 周萍等.花生壳总黄酮及木犀草素含量.《中药材》.2006,第29卷(第08期),769-771. |
| 周萍等.花生壳药材质量标准的研究.《大理学院学报》.2011,第10卷(第02期),1-3. |
| 唐丽萍等.不同产地花生壳中木犀草素的HPLC测定.《花生学报》.2005,第34卷(第02期),1--4. |
| 姚利等.花生壳中5 7-二羟基色原酮及圣草酚的HPLC测定.《食品科技》.2006 |
| 花生壳中5,7-二羟基色原酮及圣草酚的HPLC测定;姚利等;《食品科技》;20060331(第03期);116-118 * |
| 花生壳总黄酮及木犀草素含量;周萍等;《中药材》;20060831;第29卷(第08期);769-771 * |
| 花生壳药材质量标准的研究;周萍等;《大理学院学报》;20110228;第10卷(第02期);1-3 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102253145A (en) | 2011-11-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103018371B (en) | Quality control method of sunset abelmoschus root medicinal material as well as extract and preparation of sunset abelmoschus root | |
| CN105717229B (en) | A kind of method for determining 11 kinds of flavones ingredients in vine tea simultaneously with HPLC | |
| CN102928523A (en) | Wild chrysanthemum flower fingerprint determination method, its application, and wild chrysanthemum flower quality detection method | |
| CN106442789A (en) | Establishment and active component quantitative analysis methods of compound Xuezhining extract fingerprint map | |
| CN105353053A (en) | Content determination method for scutellarin and scutellarein in sculellaria barbata medicinal material and formula granule of sculellaria barbata medicinal material | |
| CN104502485B (en) | The quantitative analysis method of 6 chemical compositions in the compound Chinese medicinal preparation that is medicinal material by rhizoma dioscoreae nipponicae and wilsonii | |
| CN104090040B (en) | A kind of HPLC method of quick detection Pasania cuspidata main active | |
| CN104330482B (en) | A kind of HPLC of utilization measures the method for 17 kinds of characteristic components in Folium Camelliae sinensis simultaneously | |
| CN101961405B (en) | Method for testing content of pinoresinol diglucoside in compound eucommia bark tablet | |
| CN106680403A (en) | Method for detecting dendrophenol in Dendrobium officinale | |
| CN103592391A (en) | Method for determining specnuezhenide content in Zhenqifuzheng preparation | |
| CN103698422B (en) | Method for detecting contents of baicalin, forsythin, indirubin and glycyrrhizic acid in Qingreling granules | |
| CN103575821A (en) | Detection method of 14 chemical components in Tangminling preparation | |
| CN106324167A (en) | Method for determining flavone components in radix astragali extract by UPLC (ultra performance liquid chromatography) | |
| CN109187810B (en) | Detection method of traditional Chinese medicine composition for treating rheumatoid arthritis | |
| CN102253145B (en) | Method for detecting 5,7-dyhydroxy chromone, eriodictyol and luteolin in peanut shell simultaneously | |
| CN103293261A (en) | Content determination method of rhizoma bletillae | |
| CN109932437B (en) | Detection method of pharmaceutical composition | |
| CN113759056B (en) | Characteristic spectrum of Chinese lobelia and preparation thereof and construction method thereof | |
| CN102680593B (en) | Method for detecting medicine composition promoting qi to activate blood and dispersing blood stasis | |
| CN105675734A (en) | Method for detecting oligosaccharide component content in compound salvia miltiorrhiza bge extract | |
| CN106153761A (en) | The method of 3 kinds of flavones ingredients in detection seedless roxburgh rose fruit simultaneously | |
| CN102998386A (en) | Method for measuring radix paeoniae alba diglucoside in radix paeoniae alba callus by utilizing high performance liquid chromatography | |
| CN103091437A (en) | Determination method of hesperidin content | |
| CN102735787B (en) | Novel digestion promoting tablet and its relative preparation quality detection method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: SHANDONG CHUANGXINYUAN AGRICULTURAL TECHNOLOGY DEV Free format text: FORMER OWNER: AGRICULTURAL PRODUCTS RESEARCH INSTITUTE, SHANDONG ACADEMY OF AGRICULTURAL SCIENCES Effective date: 20130513 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20130513 Address after: 250100 No. 196-1 industrial North Road, Licheng District, Shandong, Ji'nan Patentee after: Shandong Innovation Yuan Agricultural Technology Development Co.,Ltd. Address before: Industrial Road Licheng District, Ji'nan city of Shandong Province, No. 202 250100 Patentee before: Agricultural Products Research Institute, Shandong Academy of Agricultural Sciences |
|
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130123 Termination date: 20130712 |