CN1731172A - Method for measuring Schizandrol A content in climacteric syndrome-relieving tablet - Google Patents
Method for measuring Schizandrol A content in climacteric syndrome-relieving tablet Download PDFInfo
- Publication number
- CN1731172A CN1731172A CN 200510014881 CN200510014881A CN1731172A CN 1731172 A CN1731172 A CN 1731172A CN 200510014881 CN200510014881 CN 200510014881 CN 200510014881 A CN200510014881 A CN 200510014881A CN 1731172 A CN1731172 A CN 1731172A
- Authority
- CN
- China
- Prior art keywords
- schizandrin
- climacteric
- syndrome
- determination
- solution
- 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
Images
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a method for measuring the schzandrol content of the menopausal tablet, which is formed by the following steps: (1) preparing the contrasting sample solution: extracting right amount schzandrol sample and adding carbinol to prepare them into the contrasting solution; (2) preparing the supplied sample solution: extracting the menopausal tablet sample, excising the film closing sheet, precision weighting, milling and extracting them to do precision weighting, then disposing them into the conical flask with cork, adding carbinol, water-bath heating and flowing-back, cooling and filtering them by micro hole filter as the supplied sample solution; (3) adopting high efficiency liquid chromatograph to do the measuring.
Description
Technical field
The present invention relates to schizandrin Determination on content method in a kind of Chinese medicine preparation, particularly relate to a kind of schizandrin Determination on content method in the high effective liquid chromatography for measuring Chinese medicine preparation climacteric-syndrome-relieving tablet of utilizing.
Background technology
At present, along with the continuous development of the modernization of Chinese medicine, the improving constantly of pharmaceutical technology (tcd) and quality testing level, increasing advanced detecting instrument and laboratory facilities are used to the detection of Chinese patent drug quality.Simultaneously, along with the raising of people's living standard, society is also more and more higher to the quality requirements of medicine, and this will have advanced person, stable, reliable detection method that the quality of medicine is effectively controlled with regard to requiring each pharmacy corporation.Therefore, the quality standard of raising Chinese patent drug is imperative.
In addition, country encourages each pharmacy corporation and R﹠D institution to improve existing Chinese patent drug quality standard, and passes through the raising that some approach promote quality standards, for example:
1.2005 " Chinese pharmacopoeia has increased qualitative, the quantitative identification method of many Chinese crude drugs and Chinese patent drug to a year version on the basis of version in 2000;
2. in the process that medicine registrations such as new product development and old product secondary development are declared, all require on the basis of initial quality standard, to improve.
Climacteric-syndrome-relieving tablet be in the pure Chinese medicinal preparation of the treatment climacteric syndrome developed of new medicine company Lerentang Traditional Chinese Medicine Factory, Tianjin, record in " Chinese pharmacopoeia version in 2000, form by flavour of a drug such as glutinous rehmannia, RADIX POLYGONI MULTIFLORI PREPARATA, the fruit of Chinese magnoliavine, cultivated lands, have merit nourishing Yin and clearing heat, that relieving restlessness is calmed the nerves, clinically be used for the treatment of diseases such as hectic fever sweating that climacteric occurs, dizzy, tinnitus, insomnia, dysphoria, unstable blood pressure.The fruit of Chinese magnoliavine plays mental-tranquilization, arrest sweating promotes the production of body fluid for principal ingredient in the prescription.Schizandrin is one of principal ingredient in the fruit of Chinese magnoliavine, and higher because of schizandrin content in schisandra chinensis medicinal material, therefore and stable in properties, can control this product inherent quality effectively by the monitoring to schizandrin content in the climacteric-syndrome-relieving tablet.
Summary of the invention
The purpose of this invention is to provide schizandrin Determination on content method in a kind of climacteric-syndrome-relieving tablet, the present invention is the schizandrin content that utilizes in the high effective liquid chromatography for measuring climacteric-syndrome-relieving tablet, to improve the quality standard of climacteric-syndrome-relieving tablet.
Technical scheme of the present invention is summarized as follows:
Schizandrin Determination on content method in a kind of climacteric-syndrome-relieving tablet, form by following steps:
(1) it is an amount of that the schizandrin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds the solution that methyl alcohol is made 1.066 μ g/ml～10.66 μ g/ml, preferably 4.8 μ g/ml, product solution in contrast;
(2) 20 in climacteric-syndrome-relieving tablet sample is got in the preparation of need testing solution, removes film coating, and accurate the title decides, porphyrize, it is fixed to get the accurate title of powder 0.3g, puts in the 50ml tool plug conical flask, add methyl alcohol 25ml, the accurate title, decided water-bath reflux 20-90 minute, preferably 30 minutes, put and be chilled to room temperature, the accurate title, decide, supply with methyl alcohol and to subtract weight loss, miillpore filter filters, and as need testing solution, 0.45 μ m is preferably selected in the miillpore filter aperture;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and water is 30～70: 70～30, preferably 50: 50; Detect wavelength: 217nm; Flow velocity: 0.5ml/min～1.0ml/min, preferably 0.8ml/min; 20 ℃～40 ℃ of column temperatures, preferably 25 ℃, precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measures.
Advantage of the present invention is: easily and fast, specificity and favorable reproducibility, the result can be used for the quality control of climacteric-syndrome-relieving tablet accurately and reliably.
Description of drawings
Fig. 1 is the high-efficient liquid phase chromatogram of schizandrin reference substance;
Fig. 2 is the high-efficient liquid phase chromatogram of climacteric-syndrome-relieving tablet;
The high-efficient liquid phase chromatogram of the negative reference substance of Fig. 3.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
Schizandrin Determination on content method comprises the steps: in a kind of climacteric-syndrome-relieving tablet
(1) it is an amount of that the schizandrin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methyl alcohol and makes 4.8 μ g/ml, product solution in contrast;
(2) 20 in climacteric-syndrome-relieving tablet sample is got in the preparation of need testing solution, removes film coating, and accurate the title decides, porphyrize, it is fixed to get the accurate title of powder 0.3g, puts in the 50ml tool plug conical flask, add methyl alcohol 25ml, the accurate title, decide, and water-bath reflux 30 minutes is put and is chilled to room temperature, the accurate title, decide, supply with methyl alcohol and to subtract weight loss, select 0.45 μ m miillpore filter to filter, as need testing solution;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and water is 50: 50; Detect wavelength: 217nm; Flow velocity: 0.8ml/min; 25 ℃ of column temperatures, precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measures.
Embodiment 2
Schizandrin Determination on content method comprises the steps: in a kind of climacteric-syndrome-relieving tablet
(1) it is an amount of that the schizandrin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds the solution that methyl alcohol is made 1.066 μ g/ml, in contrast product solution;
(2) 20 in climacteric-syndrome-relieving tablet sample is got in the preparation of need testing solution, removes film coating, and accurate the title decides, porphyrize, it is fixed to get the accurate title of powder 0.3g, puts in the 50ml tool plug conical flask, add methyl alcohol 25ml, the accurate title, decide, and water-bath reflux 20 minutes is put and is chilled to room temperature, the accurate title, decide, supply with methyl alcohol and to subtract weight loss, miillpore filter filters, as need testing solution;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and water is 30: 70; Detect wavelength: 217nm; Flow velocity: 0.5ml/min; 20 ℃ of column temperatures, precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measures.
Embodiment 3
Schizandrin Determination on content method comprises the steps: in a kind of climacteric-syndrome-relieving tablet
(1) it is an amount of that the schizandrin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds the solution that methyl alcohol is made 10.66 μ g/ml, in contrast product solution;
(2) 20 in climacteric-syndrome-relieving tablet sample is got in the preparation of need testing solution, removes film coating, and accurate the title decides, porphyrize, it is fixed to get the accurate title of powder 0.3g, puts in the 50ml tool plug conical flask, add methyl alcohol 25ml, the accurate title, decide, and water-bath reflux 90 minutes is put and is chilled to room temperature, the accurate title, decide, supply with methyl alcohol and to subtract weight loss, miillpore filter filters, as need testing solution;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and water is 70: 30; Detect wavelength: 217nm; Flow velocity: 1.0ml/min; 40 ℃ of column temperatures, precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measures.
Embodiment 4
Accurate schizandrin reference substance (concentration is 4.8 μ l/ml) 2,4,8,12,16, the 20 μ l sample introductions of drawing of the investigation of linear relationship, measure by above-mentioned chromatographic condition, sample size with the reference substance schizandrin is a horizontal ordinate, respective peaks area integral value is an ordinate, the calculating regression equation is Y=88998.64X-3418.35, r=0.99997.Schizandrin becomes good linear relationship in 1.066～10.66 μ g/ml scopes.
Embodiment 5
Same reference substance solution is got in the precision experiment, and continuous 5 sample introductions record the peak area integrated value, and RSD (relative standard deviation) is 0.19% as a result.
Embodiment 6
Same batch sample is got in the reappearance experiment, takes by weighing 5 parts of test samples, measures according to content assaying method, and average content is 76.596 μ g/ sheets, and RSD is 2.77%, shows that this law reappearance is good, and precision is higher.
Embodiment 7
Stability experiment is got same need testing solution, and every 2 hours sample introduction 5 μ l, sample introduction was 5 times altogether, measures peak area and calculates content, and RSD is 2.20% (n=6) as a result.
Embodiment 8
The application of sample absorption method is adopted in recovery experiment, gets 5 parts in the sample of known content (255.32mg/g, every heavy 0.31g), accurately respectively adds a certain amount of schizandrin reference substance solution, measures according to content assaying method, calculates average recovery, the results are shown in Table 1.
Table 1. recovery test result
Table 1 Result of recovery test
| Sample volume (g) | Sample schizandrin content (μ g) | Schizandrin addition (μ g) | Measurement result (μ g) | The recovery (%) | Average recovery rate (%) | RSD (％) |
| 0.1523 0.1508 0.1543 0.1516 0.1533 0.1522 | 38.88 38.51 39.38 38.70 39.14 38.86 | 38.4 38.4 38.4 38.4 38.4 38.4 | 77.32 77.91 78.36 76.60 78.77 77.14 | 100.1 102.6 101.5 98.7 103.2 99.7 | 100.96 | 1.75 |
Embodiment 9
The preparation of blank liquid takes by weighing other flavour of a drug in the prescription ratio with mensuration except that the fruit of Chinese magnoliavine, make the preparation that does not contain the fruit of Chinese magnoliavine by formulation and technology, make blank liquid by the need testing solution preparation method, measurement result is seen Fig. 1 Fig. 2 and Fig. 3, illustrates that other medicinal materials and auxiliary material all do not disturb the mensuration of schizandrin.
Embodiment 10
Sample determination is got ten batches of climacteric-syndrome-relieving tablet samples (every heavy 0.31g of climacteric-syndrome-relieving tablet), is equipped with need testing solution by need testing solution preparation below legal system, two parts of need testing solutions of every batch of preparation.Accurate need testing solution, each 5 μ l of reference substance solution of drawing inject high performance liquid chromatograph, measure, and ten batch samples the results are shown in Table 2.
The measurement result of schizandrin in table 2 climacteric-syndrome-relieving tablet
Table 2 Determination of Schizandrol A in Gengnian’an Tablet
| Lot number | Schizandrin (μ g/ sheet) |
| 040901 | 73.34 |
| 040902 | 80.71 |
| 041003 | 72.09 |
| 041004 | 76.37 |
| 041105 | 73.17 |
| 041106 | 75.61 |
| 041207 | 79.57 |
| 041208 | 78.25 |
| 050109 | 74.86 |
| 050110 | 76.03 |
Discuss
Extracting method is investigated: through consulting document, schizandrin is soluble in organic solvent, having investigated methanol eddy respectively extracted 20 minutes, 30 minutes, 1 hour, chloroform refluxing extraction 1 hour, ethyl acetate ultrasonic Extraction 30 minutes, methyl alcohol ultrasonic Extraction 1 hour, it is best that the result extracts 30 minutes effects with methanol eddy, so adopt this extracting method.
Detect the selection of wavelength: the schizandrin reference substance is adopted the determined by ultraviolet spectrophotometry absorbing wavelength, is maximum absorption wavelength at 217nm, so select 217nm to measure wavelength as liquid content.
This assay method easily and fast, specificity and favorable reproducibility, the result can be used for the quality control of climacteric-syndrome-relieving tablet accurately and reliably.
Claims (7)
1. schizandrin Determination on content method in the climacteric-syndrome-relieving tablet is characterized in that being made up of following steps:
(1) it is an amount of that the schizandrin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds the solution that methyl alcohol is made 1.066 μ g/ml～10.66 μ g/ml, in contrast product solution;
(2) 20 in climacteric-syndrome-relieving tablet sample is got in the preparation of need testing solution, removes film coating, and accurate the title decides, porphyrize, it is fixed to get the accurate title of powder 0.3g, puts in the 50ml tool plug conical flask, add methyl alcohol 25ml, the accurate title, decide, and water-bath reflux 20-90 minute is put and is chilled to room temperature, the accurate title, decide, supply with methyl alcohol and to subtract weight loss, miillpore filter filters, as need testing solution;
(3) adopt high performance liquid chromatograph to measure, chromatographic condition is: Diamonsil chromatographic column: C
18Reverse-phase chromatographic column specification: 5 μ m, 250 * 4.6mm; Moving phase: the volume ratio of acetonitrile and water is 30～70: 70～30; Detect wavelength: 217nm; Flow velocity: 0.5ml/min～1.0ml/min; 20 ℃～40 ℃ of column temperatures, precision is got reference substance solution and each 5ul of need testing solution respectively, injects described high performance liquid chromatograph, measures.
2. schizandrin Determination on content method in a kind of climacteric-syndrome-relieving tablet according to claim 1, the concentration that it is characterized in that described reference substance solution are 4.8 μ g/ml.
3. schizandrin Determination on content method in a kind of climacteric-syndrome-relieving tablet according to claim 1 is characterized in that the described need testing solution water-bath reflux time is 30 minutes.
4. schizandrin Determination on content method in a kind of climacteric-syndrome-relieving tablet according to claim 1 is characterized in that described miillpore filter aperture is 0.45 μ m.
5. schizandrin Determination on content method in a kind of climacteric-syndrome-relieving tablet according to claim 1 is characterized in that the acetonitrile in the described chromatographic condition and the volume ratio of water are 50: 50.
6. schizandrin Determination on content method in a kind of climacteric-syndrome-relieving tablet according to claim 1 is characterized in that the flow velocity in the described chromatographic condition is 0.8ml/min.
7. schizandrin Determination on content method in a kind of climacteric-syndrome-relieving tablet according to claim 1 is characterized in that the column temperature in the described chromatographic condition is 25 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100148813A CN100368802C (en) | 2005-08-26 | 2005-08-26 | Method for measuring Schizandrol A content in climacteric syndrome-relieving tablet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100148813A CN100368802C (en) | 2005-08-26 | 2005-08-26 | Method for measuring Schizandrol A content in climacteric syndrome-relieving tablet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1731172A true CN1731172A (en) | 2006-02-08 |
| CN100368802C CN100368802C (en) | 2008-02-13 |
Family
ID=35963566
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100148813A Active CN100368802C (en) | 2005-08-26 | 2005-08-26 | Method for measuring Schizandrol A content in climacteric syndrome-relieving tablet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100368802C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104062365A (en) * | 2013-03-19 | 2014-09-24 | 石家庄以岭药业股份有限公司 | Determination method of content of schisandrin in medicament |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0717554B2 (en) * | 1986-07-23 | 1995-03-01 | 株式会社ツムラ | Novel lignan derivative and antiulcer agent containing the same as active ingredient |
| CN1621836A (en) * | 2004-12-13 | 2005-06-01 | 贵阳云岩西创药物科技开发有限公司 | Quality controlling method for pulse restoring injection |
-
2005
- 2005-08-26 CN CNB2005100148813A patent/CN100368802C/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104062365A (en) * | 2013-03-19 | 2014-09-24 | 石家庄以岭药业股份有限公司 | Determination method of content of schisandrin in medicament |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100368802C (en) | 2008-02-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105467023B (en) | A kind of method that UPLC measures Herba Andrographitis medicinal materials fingerprint and four kinds of diterpenoid-lactones | |
| CN107064322B (en) | HPLC wavelength switching method for simultaneously measuring contents of gallic acid and sanguisorbin I in sanguisorba or sanguisorba preparations | |
| CN1141575C (en) | Red sage medicine fingerprint establishing method and standard fingerprint atlas | |
| CN113252821A (en) | Method for establishing fingerprint of flavonoid component in ginkgo leaf extraction intermediate or preparation thereof and established fingerprint | |
| CN102441057B (en) | High performance liquid chromatography (HPLC) fingerprint detection method for blood-nourishing brain-refreshing grain | |
| CN101029889A (en) | Method for inspecting Chinese medicinal preparation quality in treatment of old man eyes dieases | |
| CN102397517A (en) | Quality control method of traditional Tibetan medicinal lipid lowering preparation | |
| CN103245737A (en) | Detection method of anti-viral oral liquid | |
| CN102707006B (en) | Quality detection method of cudrania tricuspidata formula granules | |
| CN110530990B (en) | Detection method of caesalpinia-caesalpinia cold mixture | |
| CN101961405A (en) | Method for testing content of pinoresinol diglucoside in compound eucommia bark tablet | |
| CN116879424A (en) | Method for measuring content of terprivet glycoside in shengxuebao preparation | |
| CN103543222A (en) | Reduning injection saccharide content detection method | |
| CN1731172A (en) | Method for measuring Schizandrol A content in climacteric syndrome-relieving tablet | |
| CN113820411A (en) | Method for measuring contents of schizandrol A and schizandrol B in preparation for strengthening body resistance and removing blood stasis | |
| CN100350242C (en) | Determination method of naringoside content in stomach intestine calm pill | |
| CN110687219B (en) | Detection method of suhuang cough-relieving capsule fingerprint and application thereof | |
| CN101008632A (en) | Standard HPLC fingerprint of schisandra fruit decoction and establishing method therefor | |
| CN103837627A (en) | Fingerprint spectrum establishment method of groundnut stem and leaf medicinal material | |
| CN113341007A (en) | Method for measuring contents of multiple components in whole Chinese date seed nerve-soothing capsule based on HPLC (high performance liquid chromatography) characteristic spectrum | |
| CN102068599B (en) | Detection method for phlegm eliminating and asthma relieving cough syrup | |
| CN101530480A (en) | Quality inspection method for quick-acting cardiac pain spray | |
| CN101029890A (en) | Method for inspecting Chinese-medicinal preparation Kaiyinwan | |
| CN115541773A (en) | Detection method for 5 rhubarb anthraquinone components in traditional Chinese medicine composition for treating nephropathy | |
| CN101461859B (en) | Method for controlling quality of anti-inflammation antibacterial medicament |
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 | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 300380 Yumen Road, Xiqing District, Tianjin Patentee after: Lerentang Pharmaceutical Factory of Jinyao Darentang Group Co.,Ltd. Address before: 300380 Yumen Road, Xiqing District, Tianjin Patentee before: Letrentang pharmaceutical factory of Tianjin Zhongxin Pharmaceutical Group Co.,Ltd. |