CN104892701A - Method used for extracting hesperidin from pills used for promoting digestion - Google Patents
Method used for extracting hesperidin from pills used for promoting digestion Download PDFInfo
- Publication number
- CN104892701A CN104892701A CN201510242771.6A CN201510242771A CN104892701A CN 104892701 A CN104892701 A CN 104892701A CN 201510242771 A CN201510242771 A CN 201510242771A CN 104892701 A CN104892701 A CN 104892701A
- Authority
- CN
- China
- Prior art keywords
- extraction
- hesperidin
- lenitive pill
- described step
- lenitive
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Extraction Or Liquid Replacement (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a method used for extracting hesperidin from pills used for promoting digestion. The method comprises following steps: step 1, the pills used for promoting digestion are smashed and are mixed with diatomite; step 2, ASE extraction is adopted for extracting hesperidin, and an obtained extract is collected, wherein methyl alcohol is taken as an extracting solvent; and step 3, the extract is diluted to a constant volume, and then is subjected to filtration so as to obtain a liquid supernatant containing hesperidin. The method used for extracting hesperidin from the pills used for promoting digestion is rapid and high in accuracy.
Description
Technical field
The present invention relates to technical field of chemical detection, particularly a kind of method extracting Hesperidin from lenitive pill.
Background technology
Lenitive pill makes large honeyed bolus by Fructus Crataegi (parched to brown), Medicated Leaven (stir-fry), Ternate Pinellia (system), Poria cocos, dried orange peel, the capsule of weeping forsythia, stir-baked SEMEN RAPHANI, roasted malt eight taste processing of crude drugs
[1].Have and help digestion, lead function that is stagnant and stomach, cure mainly dyspepsia and stagnate, distension and fullness in the abdomen, rotten acid regurgitation, loss of appetite
[2].Hesperidin is one of principle active component of lenitive pill, and 2010 editions " Chinese Pharmacopoeia " is using Hesperidin as the index of quality evalution.The assay of primary standard adopts soxhlet extraction return time long, needs to consume a large amount of solvents;
Summary of the invention
The object of this invention is to provide a kind ofly to extract rapidly, precision is high, solvent load the is few method extracting Hesperidin from lenitive pill.
Technical scheme provided by the invention is: a kind of method extracting Hesperidin from lenitive pill, comprises the following steps:
Step 1: mix with diatomite after lenitive pill is pulverized; Wherein, in the lenitive pill after pulverizing, powder and diatomaceous weight ratio are 1:1;
Step 2: adopt ASE extraction process extraction Hesperidin, collect extraction liquid, wherein, the extraction solvent that ASE extraction process adopts is methyl alcohol;
Step 3: will filter after extraction liquid constant volume and obtain the extraction liquid containing Hesperidin.
Extract from above-mentioned lenitive pill in the method for Hesperidin, in described step 2, extraction temperature is 90-120 DEG C.
Extract from above-mentioned lenitive pill in the method for Hesperidin, in described step 2, extraction time is 5-10min.
Extract from above-mentioned lenitive pill in the method for Hesperidin, in described step 2, the flush volume of ASE extraction process is more than or equal to the volume of 100% abstraction pool.
Extract from above-mentioned lenitive pill in the method for Hesperidin, in described step 2, extraction cycle number of times is more than or equal to 2 times.
Extract from above-mentioned lenitive pill in the method for Hesperidin, in described step 2, adopt ASE350 type accelerated solvent extraction to carry out the operation of ASE extraction process, the system pressure of setting ASE350 type accelerated solvent extraction is 1700psi, and the nitrogen purging time is 60s.
Extract from above-mentioned lenitive pill in the method for Hesperidin, in described step 3, extraction liquid is settled to 25ml, shakes up rear filtration and namely obtains extraction liquid containing Hesperidin.
The present invention is after employing technique scheme, and its beneficial effect had is:
The present invention adopts and accelerates the extraction efficiency that abstraction technique effectively can improve Hesperidin in lenitive pill, and ensures higher accuracy rate, reduce extraction solvent consumption, and this extracting method can not produce any detrimentally affect to detection below.
Accompanying drawing explanation
Fig. 1 is the test spectrogram of embodiments of the invention 1;
Fig. 2 is the test spectrogram of standard of the present invention;
Fig. 3 is the test spectrogram of comparative example 1 of the present invention.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1:
Instrument used by the present embodiment and consumptive material are: pulverizer, electronic analytical balance (XA205DU): sensibility reciprocal 0.001g, accelerated solvent extraction model: ASE-350 (10ml abstraction pool, 50ml receiving flask), volumetric flask: 25ml.
The present embodiment lenitive pill used has been Foshan Feng sex medicine company limited produces, lot number: 140001.
Add diatomite 1.0g in abstraction pool, precision takes powder in lenitive pill (140001) and is about 0.5g, adds diatom 0.5g and mixes in rearmounted 5ml abstraction pool; The selection of Accelerate solvent extraction condition: temperature: 120 DEG C, flush volume: 100%, static extracting time: 5 minutes, cycle index: 2 times.Solvent: methyl alcohol, after extraction terminates, is transferred in 25ml volumetric flask by extraction liquid, be settled to scale, shake up with methanol dilution, filters, gets subsequent filtrate, to obtain final product.
The preparation of standard
Precision takes Hesperidin reference substance 19.45mg, be placed in 250ml measuring bottle, be diluted to scale with dissolve with methanol (if desired supersound process), shake up (namely Hesperidin concentration is 74.14 μ g/ml), precision measures 5ml, puts in 10ml measuring bottle, is diluted to scale by moving phase, shake up, obtain (every 1ml is containing Hesperidin 37.07 μ g).
Comparative example 1
This comparative example is the method for pharmacopeia record, be specially: get lenitive pill (140001), shred, mixing, get about 2.5g, accurately weighed, add diatomite appropriate, grind well, be placed in apparatus,Soxhlet's, add sherwood oil (60 DEG C-90 DEG C) 80ml, reflux 2-3 hour, discard sherwood oil, the dregs of a decoction volatilize, add methyl alcohol 80ml, reflux is to extracting liquid colourless, let cool, filter, filtrate is put in 100ml measuring bottle, with a small amount of methyl alcohol gradation washing container, washing lotion is filtered in same measuring bottle, add methyl alcohol to scale, shake up, add moving phase to scale, shake up, obtain.
Detect
Adopt U-3000 liquid chromatograph to detect, detect parameters is:
Chromatographic column: kinete x2.6 μ XB-C18100A 100 × 4.60mm post, moving phase: methyl alcohol-7% acetic acid (37:63), flow velocity: 0.7ml/min, column temperature: 40 DEG C, determined wavelength: 283nm, sample size: 5 μ l.
Following Fig. 1 and Fig. 2 of detected result of embodiment 1 and standard.Fig. 3 is the spectrogram that comparative example 1 obtains, and the sample of present method resulting separation can obtain collection of illustrative plates complete clearly, and the sample test spectrogram obtained with the separation method of comparative example 1 has height repeatability.
Embodiment 2
The present embodiment is identical with the step of embodiment 1, and different places is, has investigated extraction efficiency in the scope of 85-120 DEG C.Concrete outcome sees the following form table 1.
Table 1 temperature affects extraction yield result table
Embodiment 3
The present embodiment is identical with the step of embodiment 1, and different places is, in the scope of the cycle index of 1-4 time, investigated extraction efficiency.Concrete outcome sees the following form table 2.
Table 2 cycle index affect table
| Classification | 1 time | 2 times | 3 times | 4 times |
| Content/(mg/ ball) | 3.20 | 18.31 | 20.51 | 20.51 |
Embodiment 4
The present embodiment is identical with the step of embodiment 1, and different places is, in the scope of the static extracting time of 3-10min, investigated extraction efficiency.Concrete outcome sees the following form table 3.
The table 3 static extracting time affect table
| Time | 3min | 5min | 7min | 10min |
| Content/(mg/ ball) | 5.45 | 18.28 | 20.51 | 20.51 |
Embodiment 5
The present embodiment is identical with the step of embodiment 1, and different places is, in the scope being equivalent to the flush volume of abstraction pool volume of 0-150%, investigated extraction efficiency.Concrete outcome sees the following form table 3.
Table 4 flush volume affect table
| Flush volume | 0 | 40％ | 80％ | 100％ | 120％ | 150％ |
| Content/(mg/ ball) | 18.01 | 18.18 | 18.29 | 18.31 | 18.31 | 18.31 |
Can be found out by embodiment 2-5, consider from operating time and cost angle, the optimized parameter of ASE extraction process of the present invention is as embodiment 1.
The impact that other experiment conditions detect HPLC
1, the investigation of linearity range
Draw above-mentioned standard solution (concentration: 74.14 μ g/ml) respectively, be diluted to 3.707 μ g/ml, 18.535 μ g/ml, 37.070 μ g/ml, 55.605 μ g/ml, 74.140 μ g/ml respectively, inject HPLC instrument to measure, with reference substance concentration for X-coordinate, take peak area as ordinate zou, drawing standard curve, carries out linear regression.Hesperidin concentration is good with peak area linear relationship within the scope of 3.707 ~ 74.14 μ g/ml, and regression equation is: Y=14.421X-7.4373, R
2=0.9998.
2, solvent is on the impact of experiment
Get the negative control sample of scarce lenitive pill, negative controls solution is prepared by the method for embodiment 1, and carry out measurement result by the chromatographic condition of above-mentioned detection method and to show in negative control on the position identical with Hesperidin, without absorption peak, to show that solvent is to the negative interference of this product assay.
3, circulation ratio test
Get same sample lots, by the method described in embodiment 1, prepare 6 parts of need testing solutions, carry out measurement result by the chromatographic condition of above-mentioned detection method, the RSD calculating Hesperidin is 1.0%.As shown in table 5, result shows, this test method circulation ratio is good.
Table 5 reproducible test results
Present method separation accuracy is high, reproducible, and the used time is short, is conducive to the operation of Simplified analysis personnel.
Above-describedly be only preferred embodiment of the present invention, all do within the scope of the spirit and principles in the present invention any amendment, equivalently to replace and improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. from lenitive pill, extract a method for Hesperidin, it is characterized in that, comprise the following steps:
Step 1: mix with diatomite after lenitive pill is pulverized; Wherein, in the lenitive pill after pulverizing, powder and diatomaceous weight ratio are 1:1;
Step 2: adopt ASE extraction process extraction Hesperidin, collect extraction liquid, wherein, the extraction solvent that ASE extraction process adopts is methyl alcohol;
Step 3: will filter after extraction liquid constant volume and obtain the extraction liquid containing Hesperidin.
2. the method extracting Hesperidin from lenitive pill according to claim 1, is characterized in that, in described step 2, extraction temperature is 90-120 DEG C.
3. the method extracting Hesperidin from lenitive pill according to claim 2, is characterized in that, in described step 2, extraction time is 5-10min.
4. the method extracting Hesperidin from lenitive pill according to claim 3, is characterized in that, in described step 2, the flush volume of ASE extraction process is more than or equal to the volume of 100% abstraction pool.
5. the method extracting Hesperidin from lenitive pill according to claim 4, is characterized in that, in described step 2, extraction cycle number of times is more than or equal to 2 times.
6. the method extracting Hesperidin from lenitive pill according to claim 5, it is characterized in that, in described step 2, ASE350 type accelerated solvent extraction is adopted to carry out the operation of ASE extraction process, the system pressure of setting ASE350 type accelerated solvent extraction is 1700psi, and the nitrogen purging time is 60s.
7. the method extracting Hesperidin from lenitive pill according to claim 6, is characterized in that, in described step 3, extraction liquid is settled to 25ml, shakes up rear filtration and namely obtains extraction liquid containing Hesperidin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510242771.6A CN104892701B (en) | 2015-05-12 | 2015-05-12 | The method that aurantiamarin is extracted from Pachyma Compound Digestive Tonic Pill |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510242771.6A CN104892701B (en) | 2015-05-12 | 2015-05-12 | The method that aurantiamarin is extracted from Pachyma Compound Digestive Tonic Pill |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104892701A true CN104892701A (en) | 2015-09-09 |
| CN104892701B CN104892701B (en) | 2018-05-08 |
Family
ID=54025710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510242771.6A Active CN104892701B (en) | 2015-05-12 | 2015-05-12 | The method that aurantiamarin is extracted from Pachyma Compound Digestive Tonic Pill |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104892701B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105924489A (en) * | 2016-04-26 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for extracting platycodin in Radix Platycodonis through ASE |
| CN106924990A (en) * | 2017-04-11 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method of magnelin in ASE methods extraction flower bud of lily magnolia |
| CN107014927A (en) * | 2017-04-17 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine Determination of hesperidin in pericarpium citri reticulatae |
-
2015
- 2015-05-12 CN CN201510242771.6A patent/CN104892701B/en active Active
Non-Patent Citations (4)
| Title |
|---|
| 张卫莲； 刘燕；: "《保和丸含量测定提取工艺的研究》", 《内蒙古中医药》 * |
| 朱静: "《高效液相色谱法测定保和丸中橙皮苷的含量》", 《临床合理用药》 * |
| 郑创钦: "《加速溶剂萃取技术在中药有效成分分析中的应用》", 《中国医药导刊》 * |
| 陈军辉: "《加速溶剂萃取技术在中药有效成分分析中的应用》", 《色谱》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105924489A (en) * | 2016-04-26 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for extracting platycodin in Radix Platycodonis through ASE |
| CN106924990A (en) * | 2017-04-11 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method of magnelin in ASE methods extraction flower bud of lily magnolia |
| CN107014927A (en) * | 2017-04-17 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine Determination of hesperidin in pericarpium citri reticulatae |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104892701B (en) | 2018-05-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103336078B (en) | Method for measuring content of cough-relieving and anti-asthma pill | |
| CN104713957B (en) | A kind of assay method of root of fangji Caulis Sinomenii extract finger-print | |
| CN102928523B (en) | Wild chrysanthemum flower fingerprint determination method, its application, and wild chrysanthemum flower quality detection method | |
| CN103235082B (en) | Method for detecting Jingwu capsule | |
| CN104306745A (en) | Quality control method for rhizoma gastrodiae capsule | |
| CN103800523A (en) | Method for preparing anti-virus traditional Chinese medicinal composition and finger-print detection method | |
| CN104892701A (en) | Method used for extracting hesperidin from pills used for promoting digestion | |
| CN100437112C (en) | Method for inspecting Chinese medicinal preparation quality in treatment of old man eyes dieases | |
| CN110907550B (en) | Method for simultaneously detecting contents of six components in infant lung-ventilating and cough-relieving granules | |
| CN102441057B (en) | High performance liquid chromatography (HPLC) fingerprint detection method for blood-nourishing brain-refreshing grain | |
| CN102397517A (en) | Quality control method of traditional Tibetan medicinal lipid lowering preparation | |
| CN106324167B (en) | Method for determining flavonoid components in astragalus extract by UPLC | |
| CN101721475A (en) | Quality control method for Yaotongning capsules | |
| CN103698422B (en) | Method for detecting contents of baicalin, forsythin, indirubin and glycyrrhizic acid in Qingreling granules | |
| CN105510452B (en) | Multi-target ingredient assay, fingerprint map construction and the preparation method of liver-benefiting eye-brightening oral liquid | |
| CN104569200A (en) | Measuring method for stephania tetrandra s. moore fingerprint spectrum | |
| CN105067725B (en) | It is a kind of at the same determine shenmei stomach nourishing granule in the root of herbaceous peony, radix glycyrrhizae and the red sage root content method | |
| CN101028474B (en) | Method for inspecting the quality of Chinese preparation with Yang-and kidney tonifying functions | |
| CN111351883B (en) | Method for measuring rutin content in Sophora japonica and radix scutellariae ointment | |
| CN113820411A (en) | Method for measuring contents of schizandrol A and schizandrol B in preparation for strengthening body resistance and removing blood stasis | |
| CN108614066A (en) | A kind of Traditional Chinese medicine composition detection method for treating coronary heart disease | |
| CN105929080A (en) | Detection method of traditional Chinese medicine preparation for treating nerve-root type cervical spondylosis | |
| CN102735787B (en) | Novel digestion promoting tablet and its relative preparation quality detection method | |
| CN111579693A (en) | Method for measuring content of main effective components in antiviral cold traditional Chinese medicine preparation | |
| CN101112424A (en) | Quality control method of asthma tablets |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 543000 198 West Ring Road, Wuzhou, the Guangxi Zhuang Autonomous Region Patentee after: WUZHOU FOOD AND DRUG INSPECTION INSTITUTE Address before: 543000 198 West Ring Road, Wuzhou, the Guangxi Zhuang Autonomous Region Patentee before: WUZHOU INSTITUTE FOR FOOD AND DRUG CONTROL, GUANGXI ZHUANG AUTONOMOUS REGION |
|
| CP01 | Change in the name or title of a patent holder | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20150909 Assignee: GUANGXI GUILIN RUIDE DETECTION AUTHENTICATION TECHNOLOGY Co.,Ltd. Assignor: WUZHOU FOOD AND DRUG INSPECTION INSTITUTE Contract record no.: X2022450000291 Denomination of invention: A Method of Extracting Hesperidin from Baohe Pills Granted publication date: 20180508 License type: Common License Record date: 20221214 |
|
| EE01 | Entry into force of recordation of patent licensing contract |