CN101129471A - Quality control method of south schizandrol extract oral solid formulated product - Google Patents
Quality control method of south schizandrol extract oral solid formulated product Download PDFInfo
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- CN101129471A CN101129471A CNA2007101473680A CN200710147368A CN101129471A CN 101129471 A CN101129471 A CN 101129471A CN A2007101473680 A CNA2007101473680 A CN A2007101473680A CN 200710147368 A CN200710147368 A CN 200710147368A CN 101129471 A CN101129471 A CN 101129471A
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Abstract
The invention relates to a method for detecting dissolving rate of oral administration solid preparation which is prepared by using schisandra fruit extract as the active constituent, wherein ethanol solution, or thin hydrochloric acid or water is used as the dissolving out medium, and high performance liquid phase chromatographic method is employed to detect the dissolving quantity of Deoxyschizandrin in the oral administration solid preparation of schizandrol extract.
Description
Technical field
The present invention relates to the Fructus Schisandrae Sphenantherae ethanol extractum is the dissolution detection method of oral solid formulation of active component preparation, it is characterized in that with alcoholic solution or dilute hydrochloric acid solution or water be dissolution medium, adopt high performance liquid chromatography to detect the method for deoxyschizandrin stripping quantity in Fructus Schisandrae Sphenantherae ethanol extractum's oral solid formulation.
Background technology
Fructus Schisandrae Sphenantherae ethanol extractum oral solid formulation system is the oral solid formulations such as drop pill, capsule, tablet, pill, pellet, granule, dry suspension of active component preparation through the Fructus Schisandrae Sphenantherae ethanol extractum that decocting boils, alcohol reflux is made with the dry mature fruit Fructus Schisandrae Sphenantherae of Magnoliacea plant schisandra chinensis SchisandraSphenanthera Rehd.et Wils, have the effect that reduces serum alanine aminotransferase, be used for transaminase rising person.One of main component in the Fructus Schisandrae Sphenantherae ethanol extractum is a deoxyschizandrin, and therefore, the stripping quantity of deoxyschizandrin in the control Fructus Schisandrae Sphenantherae ethanol extractum oral solid formulation is for guaranteeing that constant product quality is controlled and clinical efficacy is significant.But existing Fructus Schisandrae Sphenantherae ethanol extractum's oral solid formulation national drug quality standard does not all record the dissolution test project at present, does not see correlational study report and Patent document data yet.
Summary of the invention
The invention provides a kind of is the method that dissolution medium, high performance liquid chromatography detect deoxyschizandrin stripping quantity in Fructus Schisandrae Sphenantherae ethanol extractum's oral solid formulation with alcoholic solution or dilute hydrochloric acid solution or water, and technical scheme is as follows:
Sample thief, according to dissolution method (two appendix XC of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine), be dissolution medium with water or dilute hydrochloric acid solution or alcoholic solution, rotating speed is that per minute 50～100 changes, behind certain hour, get solution and put evaporate to dryness in the water-bath, residue adds dissolve with methanol, puts in the measuring bottle, be diluted to scale with methanol, shake up, filter, get subsequent filtrate as need testing solution; It is an amount of that other gets the deoxyschizandrin reference substance, and accurate the title decides, and puts in the measuring bottle, adds an amount of ultrasonic dissolving that makes of methanol, is diluted to scale with methanol, shakes up, in contrast product solution.
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With the methanol-water is mobile phase; The detection wavelength is 250nm.
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005), the record chromatogram, by the stripping quantity of external standard method, promptly with deoxyschizandrin in the calculated by peak area Fructus Schisandrae Sphenantherae ethanol extractum oral solid formulation.
The specific embodiment
Embodiment 1
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
Get the about 10mg of deoxyschizandrin reference substance, accurate claim surely, put in the 50ml measuring bottle, it is an amount of to add methanol, ultrasonic dissolution (40KHZ power 120W), and be diluted to scale with methanol.The above-mentioned solution 3.0,4.0,5.0,6.0 of accurate absorption, 7.0ml put respectively in the 10ml measuring bottle, are diluted to scale with methanol, shake up, and make the standard solution of series concentration.Sample introduction 20 μ l write down chromatogram respectively, the results are shown in Table 1.
Table 1. deoxyschizandrin content assaying method linear relationship result of the test (n=5)
| Concentration (μ g/ml) | Peak area (A) |
| 0 61.92 82.56 103.2 123.84 144.48 | 0 1700637 2266705 2836001 3413982 4003302 |
With reference substance solution concentration is abscissa, and peak area is a vertical coordinate, calculates regression equation and gets:
A＝27660.48C-8696.78 r＝0.9999
The result shows: deoxyschizandrin is good with the chromatographic peak area linear relationship in 61.92～144.48 μ g/ml concentration ranges.
Embodiment 2
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
Getting concentration is the deoxyschizandrin reference substance solution of 100 μ g/ml, measures respectively at 0,2,4,6,8 hour under above-mentioned chromatographic condition, the results are shown in Table 2.
Table 2. deoxyschizandrin assay solution stability testing result
| Standing time (h) | Peak area (A) | Meansigma methods | RSD(％) |
| 0 2 4 6 8 | 2875628 2873518 2877602 2873083 2877774 | 2875521 | 0.08 |
The result shows: measure liquid and place in 8 hours stable.
Embodiment 3
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
The preparation of reference substance solution: it is an amount of to get the deoxyschizandrin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 100 μ g, promptly.
The preparation of need testing solution: get and accurately take by weighing a certain amount of deoxyschizandrin reference substance in the prescription ratio and mix with adjuvant, get in right amount, the accurate title, decide, and puts in the 10ml measuring bottle, it is an amount of to add methanol, supersound process (frequency 40KHZ, power 120W) 20 minutes is diluted to scale with methanol, shake up, filter, get subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, with deoxyschizandrin content in the calculated by peak area sample, compare calculate recovery rate by external standard method with inventory, the results are shown in Table 3.
Table 3. deoxyschizandrin assay recovery test result (n=9)
| Addition (mg) | The amount of recording (mg) | The response rate (%) | Average recovery rate (%) | RSD(％) |
| 8.10 | 8.09 8.09 8.07 | 99.88 99.88 99.63 | ||
| 10.02 | 10.00 10.00 10.00 | 99.80 99.80 99.80 | 99.8 | 0.10 |
| 10.92 | 10.90 10.91 10.91 | 99.82 99.91 99.91 |
The result shows: good with the deoxyschizandrin content response rate in HPLC method mensuration this product.
Embodiment 4
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
The preparation of reference substance solution: it is an amount of to get the deoxyschizandrin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 100 μ g, promptly.
The preparation of need testing solution: get and accurately take by weighing a certain amount of deoxyschizandrin reference substance in the prescription ratio and mix with adjuvant, get in right amount, the accurate title, decide, and puts in the 10ml measuring bottle, it is an amount of to add methanol, supersound process (frequency 40KHZ, power 120W) 20 minutes is diluted to scale with methanol, shake up, filter, get subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, with deoxyschizandrin content in the calculated by peak area sample, the results are shown in Table 4 by external standard method.
Table 4. deoxyschizandrin assay replica test (n=5)
Embodiment 5
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
The preparation of reference substance solution: it is an amount of to get the deoxyschizandrin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 100 μ g, promptly.
The preparation of need testing solution: get and accurately take by weighing a certain amount of deoxyschizandrin reference substance in the prescription ratio and mix with adjuvant, get in right amount, the accurate title, decide, and puts in the 10ml measuring bottle, it is an amount of to add methanol, supersound process (frequency 40KHZ, power 120W) 20 minutes is diluted to scale with methanol, shake up, filter, get subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, with deoxyschizandrin content in the calculated by peak area sample, different time repeats aforesaid operations 5 times by external standard method, and measurement result sees Table 5.
Table 5. deoxyschizandrin assay precision test (n=5)
The result shows: measure deoxyschizandrin content good reproducibility with this method, difference is little.
Embodiment 6
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
Getting Fructus Schisandrae Sphenantherae ethanol extractum's drop pill, according to dissolution method (two appendix XC of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine), is dissolution medium with water, 0.1mol/L hydrochloric acid solution, 10% alcoholic solution 100ml respectively, rotating speed is that per minute 100 changes, in the time of 30,45,60 minutes, get solution 10ml, filter, get subsequent filtrate 5ml and put evaporate to dryness in the water-bath, residue adds dissolve with methanol, puts in the 5ml measuring bottle, is diluted to scale with methanol, shake up, as need testing solution; Other gets the about 5mg of deoxyschizandrin reference substance, and accurate the title decides, and puts in the 50ml measuring bottle, adds ultrasonic in right amount (the frequency 40KHZ of methanol, power 120W) make dissolving, be diluted to scale with methanol, shake up, precision is measured 1.0ml and is put in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, in contrast product solution.
Get each 20 μ l of above-mentioned need testing solution and reference substance solution, inject chromatograph of liquid, the record chromatogram by the stripping quantity of external standard method with deoxyschizandrin in the every ball of calculated by peak area, the results are shown in Table 6.
The dissolution result of the test of table 6. Fructus Schisandrae Sphenantherae ethanol extractum drop pill in different dissolution mediums
Embodiment 7
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
Getting Fructus Schisandrae Sphenantherae ethanol extractum's drop pill, according to dissolution method (two appendix XC of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine), is dissolution medium with 15% alcoholic solution 100ml, 200ml respectively, rotating speed is that per minute 100 changes, in the time of 30,45,60 minutes, get solution 10ml, filter, get subsequent filtrate 5ml and put evaporate to dryness in the water-bath, residue adds dissolve with methanol, puts in the 5ml measuring bottle, is diluted to scale with methanol, shake up, as need testing solution; Other gets the about 5mg of deoxyschizandrin reference substance, and accurate the title decides, and puts in the 50ml measuring bottle, adds ultrasonic in right amount (the frequency 40KHZ of methanol, power 120W) make dissolving, be diluted to scale with methanol, shake up, precision is measured 1.0ml and is put in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, in contrast product solution.
Get each 20 μ l of above-mentioned need testing solution and reference substance solution, inject chromatograph of liquid, the record chromatogram by the stripping quantity of external standard method with deoxyschizandrin in the every ball of calculated by peak area, the results are shown in Table 7.
Table 7. Fructus Schisandrae Sphenantherae ethanol extractum drop pill dissolution result of the test in the dissolution medium of different volumes
Embodiment 8
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
Getting Fructus Schisandrae Sphenantherae ethanol extractum's drop pill, according to dissolution method (two appendix XC of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine), is dissolution medium with 15% alcoholic solution 100ml, rotating speed is that per minute 100 changes, in the time of 30,45,60 minutes, get solution 10ml, precision is measured 5ml and is put evaporate to dryness in the water-bath, residue adds dissolve with methanol, put in the 5ml measuring bottle, be diluted to scale, shake up with methanol, filter, get subsequent filtrate as need testing solution; Get the about 5mg of deoxyschizandrin reference substance, the accurate title, decide, and puts in the 50ml measuring bottle, adds ultrasonic in right amount (the frequency 40KHZ of methanol, power 120W) make dissolving, be diluted to scale with methanol, shake up, precision is measured 1.0ml and is put in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, in contrast product solution.
Get each 20 μ l of above-mentioned need testing solution and reference substance solution, inject chromatograph of liquid, the record chromatogram is by the stripping quantity of external standard method with deoxyschizandrin in the every ball of calculated by peak area.Accumulation stripping testing result sees Table 8,9.
The drop pill accumulation dissolution test result of table 8. Fructus Schisandrae Sphenantherae ethanol extractum
| Time (minute) | Stripping quantity (mg/ ball) | Meansigma methods (mg/ ball) | |||||
| 1 | 2 | 3 | 4 | 5 | 6 | ||
| 30 45 60 | 0.17 0.17 0.17 | 0.17 0.17 0.18 | 0.16 0.16 0.16 | 0.17 0.17 0.17 | 0.18 0.17 0.17 | 0.17 0.16 0.16 | 0.17 0.17 0.17 |
The drop pill three batch samples accumulation dissolution test result of table 9. Fructus Schisandrae Sphenantherae ethanol extractum
| Time (minute) | Stripping quantity (mg/ ball) | ||
| Sample 1 | Sample 2 | Sample 3 | |
| 30 45 60 | 0.17 0.17 0.17 | 0.19 0.18 0.19 | 0.17 0.18 0.19 |
Embodiment 9
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
Getting Fructus Schisandrae Sphenantherae ethanol extractum's drop pill, according to dissolution method (two appendix XC of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine), is dissolution medium with 15% alcoholic solution 100ml, rotating speed is that per minute 100 changes, in the time of 30,45,60 minutes, get solution 10ml, precision is measured 5ml and is put evaporate to dryness in the water-bath, residue adds dissolve with methanol, put in the 5ml measuring bottle, be diluted to scale, shake up with methanol, filter, get subsequent filtrate as need testing solution; Get the about 5mg of deoxyschizandrin reference substance, the accurate title, decide, and puts in the 50ml measuring bottle, adds ultrasonic in right amount (the frequency 40KHZ of methanol, power 120W) make dissolving, be diluted to scale with methanol, shake up, precision is measured 1.0ml and is put in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, in contrast product solution.
Get each 20 μ l of above-mentioned need testing solution and reference substance solution, inject chromatograph of liquid, the record chromatogram, by the stripping quantity of external standard method with deoxyschizandrin in the every ball of calculated by peak area, 8 batch sample testing results see Table 10.
Table 10. Fructus Schisandrae Sphenantherae ethanol extractum drop pill 8 batch sample stripping quantity testing results
| Sequence number | Stripping quantity (mg/ ball) | |||||||
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | Sample 7 | Sample 8 | |
| 123456 is average | 0.17 0.17 0.16 0.17 0.17 0.16 0.17 | 0.19 0.19 0.18 0.18 0.19 0.17 0.18 | 0.18 0.16 0.18 0.19 0.19 0.18 0.18 | 0.23 0.21 0.22 0.21 0.22 0.21 0.22 | 0.18 0.18 0.18 0.18 0.18 0.18 0.18 | 0.18 0.18 0.18 0.18 0.19 0.18 0.18 | 0.20 0.19 0.20 0.18 0.22 0.19 0.20 | 0.16 0.18 0.17 0.17 0.16 0.15 0.17 |
Embodiment 10
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
Getting Fructus Schisandrae Sphenantherae ethanol extractum's capsule, according to dissolution method (two appendix XC second methods of Chinese Pharmacopoeia version in 2005), is dissolution medium with 15% alcoholic solution 1000ml, rotating speed is that per minute 100 changes, in the time of 30,45,60 minutes, get solution 10ml, precision is measured 5ml and is put evaporate to dryness in the water-bath, residue adds dissolve with methanol, put in the 10ml measuring bottle, be diluted to scale, shake up with methanol, filter, get subsequent filtrate as need testing solution; Other gets the about 5mg of deoxyschizandrin reference substance, and accurate the title decides, and puts in the 50ml measuring bottle, adds ultrasonic in right amount (the frequency 40KHZ of methanol, power 120W) make dissolving, be diluted to scale with methanol, shake up, precision is measured 1.0ml and is put in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, in contrast product solution.
Get each 20 μ l of above-mentioned need testing solution and reference substance solution, inject chromatograph of liquid, the record chromatogram by the stripping quantity of external standard method with deoxyschizandrin in every of the calculated by peak area, the results are shown in Table 11.
Table 11. Fructus Schisandrae Sphenantherae ethanol extractum capsule stripping quantity testing result
| Time (minute) | 30 | 45 | 60 |
| Stripping quantity (mg/ grain) | 0.47 | 0.55 | 0.61 |
Embodiment 11
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
Getting Fructus Schisandrae Sphenantherae ethanol extractum's sheet, according to dissolution method (two appendix XC second methods of Chinese Pharmacopoeia version in 2005), is dissolution medium with 15% alcoholic solution 1000ml, rotating speed is that per minute 100 changes, in the time of 30,45,60 minutes, get solution 10ml, precision is measured 5ml and is put evaporate to dryness in the water-bath, residue adds dissolve with methanol, put in the 10ml measuring bottle, be diluted to scale, shake up with methanol, filter, get subsequent filtrate as need testing solution; Other gets the about 5mg of deoxyschizandrin reference substance, and accurate the title decides, and puts in the 50ml measuring bottle, adds ultrasonic in right amount (the frequency 40KHZ of methanol, power 120W) make dissolving, be diluted to scale with methanol, shake up, precision is measured 1.0ml and is put in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, in contrast product solution.
Get each 20 μ l of above-mentioned need testing solution and reference substance solution, inject chromatograph of liquid, the record chromatogram by the stripping quantity of external standard method with every middle deoxyschizandrin of calculated by peak area, the results are shown in Table 12.
Table 12. Fructus Schisandrae Sphenantherae ethanol extractum sheet stripping quantity testing result
| Time (minute) | 30 | 45 | 60 |
| Stripping quantity (mg/ sheet) | 0.43 | 0.49 | 0.50 |
Embodiment 12
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-water (70: 30) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by the deoxyschizandrin peak should be not less than 2000.
Getting Fructus Schisandrae Sphenantherae ethanol extractum's micropill, according to dissolution method (two appendix XC second methods of Chinese Pharmacopoeia version in 2005), is dissolution medium with 15% alcoholic solution 1000ml, rotating speed is that per minute 100 changes, in the time of 30,45,60 minutes, get solution 10ml, precision is measured 5ml and is put evaporate to dryness in the water-bath, residue adds dissolve with methanol, put in the 10ml measuring bottle, be diluted to scale, shake up with methanol, filter, get subsequent filtrate as need testing solution; Other gets the about 5mg of deoxyschizandrin reference substance, and accurate the title decides, and puts in the 50ml measuring bottle, adds ultrasonic in right amount (the frequency 40KHZ of methanol, power 120W) make dissolving, be diluted to scale with methanol, shake up, precision is measured 1.0ml and is put in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, in contrast product solution.
Get each 20 μ l of above-mentioned need testing solution and reference substance solution, inject chromatograph of liquid, the record chromatogram by the stripping quantity of external standard method with deoxyschizandrin in the every g sample of calculated by peak area, the results are shown in Table 13.
Table 13. Fructus Schisandrae Sphenantherae ethanol extractum micropill stripping quantity testing result
| Time (minute) | 30 | 45 | 60 |
| Stripping quantity (mg/g) | 0.21 | 0.35 | 0.28 |
Claims (3)
1. quality control method of south schizandrol extract oral solid formulated product, its feature is a sample thief in it, according to two appendix XC of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine dissolution method, with water is dissolution medium, rotating speed is that per minute 50～100 changes, and behind certain hour, gets solution and puts evaporate to dryness in the water-bath, residue adds dissolve with methanol, put in the measuring bottle, be diluted to scale, shake up with methanol, filter, get subsequent filtrate as need testing solution; It is an amount of that other gets the deoxyschizandrin reference substance, and accurate the title decides, and puts in the measuring bottle, adds an amount of ultrasonic dissolving that makes of methanol, is diluted to scale with methanol, shakes up, in contrast product solution; Chromatographic condition and system suitability test are mobile phase with the methanol-water for being filler with octadecylsilane chemically bonded silica, and the detection wavelength is 250nm; Algoscopy is drawn reference substance solution and each 20 μ l of need testing solution for difference is accurate, inject chromatograph of liquid, according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring, the record chromatogram is by the method for external standard method with the stripping quantity of deoxyschizandrin in the calculated by peak area Fructus Schisandrae Sphenantherae ethanol extractum oral solid formulation.
2. quality control method of south schizandrol extract oral solid formulated product, its feature is a sample thief in it, according to two appendix XC of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine dissolution method, with the dilute hydrochloric acid solution is dissolution medium, rotating speed is that per minute 50～100 changes, and behind certain hour, gets solution and puts evaporate to dryness in the water-bath, residue adds dissolve with methanol, put in the measuring bottle, be diluted to scale, shake up with methanol, filter, get subsequent filtrate as need testing solution; It is an amount of that other gets the deoxyschizandrin reference substance, and accurate the title decides, and puts in the measuring bottle, adds an amount of ultrasonic dissolving that makes of methanol, is diluted to scale with methanol, shakes up, in contrast product solution; Chromatographic condition and system suitability test are mobile phase with the methanol-water for being filler with octadecylsilane chemically bonded silica, and the detection wavelength is 250nm; Algoscopy is drawn reference substance solution and each 20 μ l of need testing solution for difference is accurate, inject chromatograph of liquid, according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring, the record chromatogram is by the method for external standard method with the stripping quantity of deoxyschizandrin in the calculated by peak area Fructus Schisandrae Sphenantherae ethanol extractum oral solid formulation.
3. quality control method of south schizandrol extract oral solid formulated product, its feature is a sample thief in it, according to two appendix XC of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine dissolution method, with the alcoholic solution is dissolution medium, rotating speed is that per minute 50～100 changes, and behind certain hour, gets solution and puts evaporate to dryness in the water-bath, residue adds dissolve with methanol, put in the measuring bottle, be diluted to scale, shake up with methanol, filter, get subsequent filtrate as need testing solution; It is an amount of that other gets the deoxyschizandrin reference substance, and accurate the title decides, and puts in the measuring bottle, adds an amount of ultrasonic dissolving that makes of methanol, is diluted to scale with methanol, shakes up, in contrast product solution; Chromatographic condition and system suitability test are mobile phase with the methanol-water for being filler with octadecylsilane chemically bonded silica, and the detection wavelength is 250nm; Algoscopy is drawn reference substance solution and each 20 μ l of need testing solution for difference is accurate, inject chromatograph of liquid, according to an appendix VID of Chinese Pharmacopoeia version in 2005 high effective liquid chromatography for measuring, the record chromatogram is by the method for external standard method with the stripping quantity of deoxyschizandrin in the calculated by peak area Fructus Schisandrae Sphenantherae ethanol extractum oral solid formulation.
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| CN102419350A (en) * | 2011-08-09 | 2012-04-18 | 中国科学院过程工程研究所 | Method for carrying out simultaneous quantitative analysis on four lignan components in Chinese magnoliavine raw material and Chinese magnoliavine extract |
| CN102419350B (en) * | 2011-08-09 | 2014-07-02 | 中国科学院过程工程研究所 | Method for carrying out simultaneous quantitative analysis on four lignan components in Chinese magnoliavine raw material and Chinese magnoliavine extract |
| CN104991032A (en) * | 2015-07-23 | 2015-10-21 | 北京市药品检验所 | Thin layer chromatography for identifying doped kadsura longepedunculata in Chinese magnoliavine |
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