CN101579422A - Measuring method of high-performance liquid chromatogram fingerprint of jiangzhining - Google Patents
Measuring method of high-performance liquid chromatogram fingerprint of jiangzhining Download PDFInfo
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Abstract
The invention discloses a measuring method of high-performance liquid chromatogram fingerprint of jiangzhining. The method mainly comprises the following steps of: preparation of reference object solution, preparation of test article solution, chromatographic condition, measurement and establishment of fingerprint, calculation of fingerprint similarity and method validation and the like. The established high-performance liquid chromatogram fingerprint of jiangzhining has 29 common chromatographic peaks, 2,3,5,4'-tetrahydroxystilbene-2-O-Beta-D-glucoside peak (16th peak) is adopted as a reference peak, relative retention time and relative peak area of various common peaks are calculated, wherein the number of the chromatographic peak with the unimodal area of exceeding 20 percent of total peak area is 1 (19th peak); the number of the chromatographic peaks with the unimodal area of exceeding 10 to 20 percent of total peak area is 2 (2nd peak and 16th peak); the number of the chromatographic peaks with the unimodal area of exceeding 5 to 10 percent of total peak area is 2 (10th peak and 18th peak); and the number of the chromatographic peaks with the unimodal area of exceeding 2 to 5 percent of total peak area is 4 (3rd peak, 4th peak, 14th peak and 22nd peak).
Description
Technical field
The present invention relates to a kind of assay method of Colestid finger printing, specifically use high performance liquid chromatography (HPLC) fingerprint spectrum method to estimate and control a kind of method of Colestid quality.
Background technology
Colestid records in the 13 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese medicine), is made up of Fructus Crataegi, Radix Polygoni Multiflori Preparata, Semen Cassiae, Folium Nelumbinis 4 flavor Chinese medicines, has promoting the flow of QI-blood by warming the meridian, sets upright dispelling wind, the effect of dredge the meridian passage.Modern pharmacological research shows that Colestid has blood fat reducing, vessel softening effect, and clinical use is extensive, and is evident in efficacy.But present quality control and evaluation methodology about Colestid, very simple, only have and differentiate that (employing chemical reaction discriminating alkaloid, anthraquinone and a flavone) records under the 13 Colestid item of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese medicine), level is very low, cause the clinical efficacy instability, there is hidden danger in safety.Therefore, press for and set up the rational quality evaluation system of Colestid,, guarantee that finally safety of clinical administration is effective to improve the modernization of pharmaceutical production technology, lifting drug quality, the secondary development of promotion medicine, realization medicine.The relevant patent of also not seeing relevant Colestid quality evaluating method at present.Fingerprint pattern technology be at present the middle pharmaceutically active ingredient overwhelming majority still can not be clear and definite situation under, effectively a kind of effective means of control and evaluation Chinese crude drug and Chinese patent medicine quality has embodied Chinese medicine quality control and evaluation model to development trend comprehensive, that macroscopic, quantifiable qualitative identification combines with main effectively component quantifying analysis.Quality with fingerprint spectrum method control and evaluation Colestid characterizes its quality on the whole effectively, has important academic significance and very strong practical value.
Technical scheme
The object of the present invention is to provide a kind of assay method of efficient liquid-phase chromatograph finger print atlas of Colestid.
The objective of the invention is to be achieved through the following technical solutions:
1. the preparation of object of reference solution
Precision takes by weighing 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside reference substance 3～10mg is put in 5～25mL measuring bottle, add dissolve with methanol and be diluted to scale, precision pipettes 0.5～5mL, puts in 5～25mL measuring bottle, adds 30～70% methanol and is diluted to scale, shake up, as object of reference solution.
2. the preparation of need testing solution
Take by weighing Radix Polygoni Multiflori Preparata 5g, Folium Nelumbinis 15g, 50% soak with ethanol that adds 20 times of parts by volume reflux, extract, 3 hours after 1 hour filters, and the same method of filtering residue is reflux, extract, 2 times again, is respectively 2 hours and 1 hour, merges three times filtrate, and being concentrated into does not have pure the flavor.Take by weighing Fructus Crataegi 100g, Semen Cassiae 5g, the water of 7 times of parts by volume of adding boiled 2 hours, filtered, and filtering residue adds the water of 5 times of parts by volume, boils 2 hours again, merges filtrate twice, concentrates.Alcohol is mentioned that the decocting in water concentrated solution merges, mix homogeneously, it is 500～1500mL that adding distil water is adjusted volume.Measure the above-mentioned aqueous solution of 25～100mL again thin up become 50～200mL solution as sample solution, by 25～150mLAB-8 or D101 or HPD300 type macroporous adsorptive resins, carry out eluting with 2～7 column volumes of 30～70% ethanol after washing 2～7 column volumes, collect 30～70% ethanol elution, reclaim solvent, evaporate to dryness obtains 30～70% ethanol elution parts.Get the about 10～50mg of 30～70% ethanol elution parts, the accurate title, decide, and puts in the conical flask, adds 30～70% ethanol, 5～25mL, claim to decide weight, supersound extraction 15～45min is put coldly, claims to decide weight again, supply the weight that subtracts mistake with 30～70% ethanol, shake up, 0.22 μ m or 0.45 μ m microporous filter membrane filter, and get subsequent filtrate as need testing solution.
3. chromatographic condition
Chromatographic column: Agilent TC-C
18Post (4.6mm * 250mm, 5 μ m), mobile phase: 0.01% aqueous formic acid-acetonitrile mixed solvent gradient elution (condition of gradient elution such as table 1); Flow velocity: 0.8～1.2mL/min; Detect wavelength: 275～285nm; Column temperature: 25～35 ℃.
Table 1 condition of gradient elution table
4. determining fingerprint pattern and foundation
The accurate need testing solution of drawing injects chromatograph of liquid, according to high effective liquid chromatography for measuring, obtains the Colestid finger printing.This finger printing has 29 total chromatographic peaks, selects 2,3,5, and 4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak (No. 16 peaks) is calculated each total peak relative retention time and relative peak area as with reference to the peak.Wherein:
Unimodal area surpasses 1 of the chromatographic peak of total peak area 20%: and No. 19 peaks (relative retention time 1.11～1.13, RSD is less than 1%; Relative peak area 1.73～1.76, RSD is less than 5%).
Unimodal area accounts for 2 of the chromatographic peaks of total peak area 10～20%: and No. 2 peaks (relative retention time 0.19～0.20, RSD is less than 1%; Relative peak area 1.23～1.25, RSD is less than 5%), No. 16 peaks (with reference to the peak).
Unimodal area accounts for 2 of the chromatographic peaks of total peak area 5～10%: and No. 10 peaks (relative retention time 0.50～0.52, RSD is less than 1%; Relative peak area 0.44～0.47, RSD is less than 15%), No. 18 peaks (relative retention time 1.00～1.10, RSD is less than 1%; Relative peak area 0.37～0.40, RSD is less than 15%).
Unimodal area accounts for 4 of the chromatographic peaks of total peak area 2～5%: and No. 3 peaks (relative retention time 0.22～0.24, RSD is less than 1%; Relative peak area 0.16～0.18, RSD is less than 5%), No. 4 peaks (relative retention time 0.27～0.29, RSD is less than 1%; Relative peak area 0.19～0.21, RSD is less than 5%), No. 14 peaks (relative retention time 0.68～0.71, RSD is less than 1%; Relative peak area 0.34～0.37, RSD is less than 15%), No. 22 peaks (relative retention time 1.32～1.34, RSD is less than 1%; Relative peak area 0.35～0.37, RSD is less than 10%).
5. the finger printing similarity is calculated
" Chinese medicine fingerprint similarity evaluation systematic study version (2004A) " with different lot number Colestid finger printing data importing Chinese Pharmacopoeia Commission's exploitation in 2004, calculate the similarity of the contrast collection of illustrative plates R of each sample finger printing and generation, all more than 0.9.
The checking of 6 methodologies
6.1 precision test
Accurate need testing solution 5～15 μ L that draw, continuous sample introduction 5 times is measured the HPLC collection of illustrative plates.With 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak (No. 16 peaks) is with reference to the peak, and the RSD value of calculating each total peak relative retention time is less than 2%, and the RSD value of relative peak area is less than 3%.
6.2 stability test
Accurate need testing solution 5～15 μ L that draw, respectively at preparation back 3,6,9,12,15,18, the 24h sample introduction is measured the HPLC collection of illustrative plates.With 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak (No. 16 peaks) is with reference to the peak, and the RSD value of calculating each total peak relative retention time is less than 2%, and the RSD value of relative peak area is less than 3%.Need testing solution is stable at 24h.
6.3 replica test
Get with 5 parts of a collection of medical materials, the preparation need testing solution, sample introduction is measured the HPLC collection of illustrative plates respectively.With 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak (No. 16 peaks) is with reference to the peak, and the RSD value of calculating each total peak relative retention time is less than 2%, and the RSD value of relative peak area is less than 3%.
Description of drawings:
Fig. 1 Colestid HPLC finger printing
Fig. 2 precision test HPLC chromatogram
Fig. 3 stability test HPLC chromatogram
Fig. 4 replica test HPLC chromatogram
0 crowd of Colestid HPLC of Figure 51 finger printing (with batch medical material)
0 crowd of Colestid HPLC of Figure 61 finger printing (different batches medical material)
10 batches of Colestid finger printing by same batch of medical material preparation:
1. the preparation of object of reference solution
Precision takes by weighing 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside reference substance 3.66mg, put in the 10mL measuring bottle, add dissolve with methanol and be diluted to scale, precision pipettes 1mL, puts in the 10mL measuring bottle, add 50% methanol and be diluted to scale, shake up, as object of reference solution.
2. the preparation of need testing solution
Take by weighing Radix Polygoni Multiflori Preparata 5g, Folium Nelumbinis 15g, 50% soak with ethanol that adds 20 times of parts by volume reflux, extract, 3 hours after 1 hour filters, and the same method of filtering residue is reflux, extract, 2 times again, is respectively 2 hours and 1 hour, merges three times filtrate, and being concentrated into does not have pure the flavor.Take by weighing Fructus Crataegi 100g, Semen Cassiae 5g, the water of 7 times of parts by volume of adding boiled 2 hours, filtered, and filtering residue adds the water of 5 times of parts by volume, boils 2 hours again, merges filtrate twice, concentrates.Alcohol is mentioned that the decocting in water concentrated solution merges, mix homogeneously, it is 1000mL that adding distil water is adjusted volume.Measure the above-mentioned aqueous solution of 50mL again thin up become 120mL solution as sample solution, by 50mL AB-8 type macroporous adsorptive resins, carry out eluting with 5 column volumes of 50% ethanol after washing 5 column volumes, collect 50% ethanol elution, reclaim solvent, evaporate to dryness obtains 50% ethanol elution part.Get the partly about 25mg of 50% ethanol elution, the accurate title, decide, and puts in the conical flask, adds 50% ethanol 10mL, claim decide weight, supersound extraction 30min is put coldly, and weight decided in title again, supply the weight that subtracts mistake with 50% ethanol, shake up, 0.45 μ m microporous filter membrane filters, and gets subsequent filtrate as need testing solution.
3. chromatographic condition
Chromatographic column: Agilent TC-C
18Post (4.6mm * 250mm, 5 μ m), mobile phase: 0.01% aqueous formic acid-acetonitrile mixed solvent gradient elution (condition of gradient elution such as table 2); Flow velocity: 1.0mL/min; Detect wavelength: 280nm; Column temperature: 30 ℃.
Table 2 condition of gradient elution table
4. determining fingerprint pattern and foundation
The accurate need testing solution of drawing injects chromatograph of liquid, according to high effective liquid chromatography for measuring, obtains the Colestid finger printing.This finger printing has 29 total chromatographic peaks, selects 2,3,5, and 4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak (No. 16 peaks) is calculated each total peak relative retention time and relative peak area as with reference to the peak.The results are shown in Table 3～4.
The total peak of 10 batches of Colestids of table 3 (with batch medical material) finger printing relative retention time
The total peak of 10 batches of Colestids of table 4 (with batch medical material) finger printing relative peak area
5. the finger printing similarity is calculated
With " the Chinese medicine fingerprint similarity evaluation systematic study version (2004A) " of 10 batches of Colestid finger printing data importing Chinese Pharmacopoeia Commission's exploitation in 2004, calculate the similarity of the contrast collection of illustrative plates R of each sample finger printing and generation, the results are shown in Table 5.
10 batches of Colestids of table 5 (with batch medical material) finger printing similarity analysis result
10 batches of Colestid finger printing by the preparation of different batches medical material:
1. the preparation of object of reference solution
Precision takes by weighing 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside reference substance 5.04mg, put in the 25mL measuring bottle, add dissolve with methanol and be diluted to scale, precision pipettes 2mL, puts in the 25mL measuring bottle, add 70% methanol and be diluted to scale, shake up, as object of reference solution.
2. the preparation of need testing solution
Take by weighing Radix Polygoni Multiflori Preparata 5g, Folium Nelumbinis 15g, 50% soak with ethanol that adds 20 times of parts by volume reflux, extract, 3 hours after 1 hour filters, and the same method of filtering residue is reflux, extract, 2 times again, is respectively 2 hours and 1 hour, merges three times filtrate, and being concentrated into does not have pure the flavor.Take by weighing Fructus Crataegi 100g, Semen Cassiae 5g, the water of 7 times of parts by volume of adding boiled 2 hours, filtered, and filtering residue adds the water of 5 times of parts by volume, boils 2 hours again, merges filtrate twice, concentrates.Alcohol is mentioned that the decocting in water concentrated solution merges, mix homogeneously, it is 1200mL that adding distil water is adjusted volume.Measure the above-mentioned aqueous solution of 80mL again thin up become 150mL solution as sample solution, by 120mL D101 type macroporous adsorptive resins, carry out eluting with 4 column volumes of 70% ethanol after washing 6 column volumes, collect 70% ethanol elution, reclaim solvent, evaporate to dryness obtains 70% ethanol elution part.Get the partly about 30mg of 70% ethanol elution, the accurate title, decide, and puts in the conical flask, adds 70% ethanol 25mL, claim decide weight, supersound extraction 40min is put coldly, and weight decided in title again, supply the weight that subtracts mistake with 70% ethanol, shake up, 0.22 μ m microporous filter membrane filters, and gets subsequent filtrate as need testing solution.
3. chromatographic condition
Chromatographic column: Agilent TC-C
18Post (4.6mm * 250mm, 5 μ m), mobile phase: 0.01% aqueous formic acid-acetonitrile mixed solvent gradient elution (condition of gradient elution such as table 6); Flow velocity: 1.2mL/min; Detect wavelength: 278nm; Column temperature: 25 ℃.
Table 6 condition of gradient elution table
4. determining fingerprint pattern and foundation
The accurate need testing solution of drawing injects chromatograph of liquid, according to high effective liquid chromatography for measuring, obtains the Colestid finger printing.This finger printing has 29 total chromatographic peaks, selects 2,3,5, and 4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak (No. 16 peaks) is calculated each total peak relative retention time and relative peak area as with reference to the peak.The results are shown in Table 7,8.
The total peak of 10 batches of Colestids of table 7 (different batches medical material) finger printing relative retention time
The total peak of 10 batches of Colestids of table 8 (different batches medical material) finger printing relative peak area
5. the finger printing similarity is calculated
With " the Chinese medicine fingerprint similarity evaluation systematic study version (2004A) " of 10 batches of Colestid finger printing data importing Chinese Pharmacopoeia Commission's exploitation in 2004, calculate the similarity of the contrast collection of illustrative plates R of each sample finger printing and generation, the results are shown in Table 9.
10 batches of Colestids of table 9 (different batches medical material) finger printing similarity analysis result
Claims (7)
1. the efficient liquid-phase chromatograph finger print atlas assay method of a Colestid, it is characterized in that comprising preparation, the need testing solution of object of reference solution preparation, chromatographic condition, finger printing mensuration and foundation, finger printing similarity are calculated and key steps such as methodology checking.
2. the assay method of Colestid efficient liquid-phase chromatograph finger print atlas as claimed in claim 1, the preparation method that it is characterized in that object of reference solution is: precision takes by weighing 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside reference substance 3～10mg, put in 5～25mL measuring bottle, add dissolve with methanol and be diluted to scale, precision pipettes 0.5～5mL, puts in 5～25mL measuring bottle, add 30～70% methanol and be diluted to scale, shake up as object of reference solution.
3. the assay method of Colestid efficient liquid-phase chromatograph finger print atlas as claimed in claim 1, the preparation method that it is characterized in that need testing solution is: take by weighing Radix Polygoni Multiflori Preparata 5g, Folium Nelumbinis 15g, 50% soak with ethanol that adds 20 times of parts by volume reflux, extract, 3 hours after 1 hour, filter, the same method of filtering residue is reflux, extract, 2 times again, is respectively 2 hours and 1 hour, merge three times filtrate, being concentrated into does not have the alcohol flavor; Take by weighing Fructus Crataegi 100g, Semen Cassiae 5g, the water of 7 times of parts by volume of adding boiled 2 hours, filtered, and filtering residue adds the water of 5 times of parts by volume, boils 2 hours again, merges filtrate twice, concentrates; Alcohol is mentioned that the decocting in water concentrated solution merges, mix homogeneously, it is 500～1500mL that adding distil water is adjusted volume; Measure the above-mentioned aqueous solution of 25～100mL again thin up become 50～200mL solution as sample solution, by 25～150mL AB-8 or D101 or HPD300 type macroporous adsorptive resins, carry out eluting with 2～7 column volumes of 30～70% ethanol after washing 2～7 column volumes, collect 30～70% ethanol elution, reclaim solvent, evaporate to dryness obtains 30～70% ethanol elution parts; Get the about 10～50mg of 30～70% ethanol elution parts, the accurate title, decide, and puts in the conical flask, adds 30～70% ethanol, 5～25mL, claim to decide weight, supersound extraction 15～45min is put coldly, claims to decide weight again, supply the weight that subtracts mistake with 30～70% ethanol, shake up, 0.22 μ m or 0.45 μ m microporous filter membrane filter, and get subsequent filtrate as need testing solution.
4. the assay method of Colestid efficient liquid-phase chromatograph finger print atlas as claimed in claim 1 is characterized in that high-efficient liquid phase chromatogram condition is: mobile phase is 0.01% aqueous formic acid-acetonitrile mixed solvent gradient elution (0 → 40min, 97: 3 → 86: 14; 40 → 65min, 86: 14 → 84: 16; 65 → 100min, 84: 16 → 70: 30; 100 → 110min, 70: 30 → 50: 50; 110 → 120min, 50: 50 → 0: 100; 120 → 130min, 0: 100 → 0: 100); Flow velocity is 0.8～1.2mL/min, and the detection wavelength is 275～285nm; Column temperature is 25～35 ℃.
5. the assay method of Colestid efficient liquid-phase chromatograph finger print atlas as claimed in claim 1, it is characterized in that the Colestid efficient liquid-phase chromatograph finger print atlas has 29 total chromatographic peaks, with 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak (No. 16 peaks) is with reference to the peak, calculates each total peak relative retention time and relative peak area; Wherein:
Unimodal area surpasses 1 of the chromatographic peak of total peak area 20%: and No. 19 peaks (relative retention time 1.11～1.13, RSD is less than 1%; Relative peak area 1.73～1.76, RSD is less than 5%);
Unimodal area accounts for 2 of the chromatographic peaks of total peak area 10～20%: and No. 2 peaks (relative retention time 0.19～0.20, RSD is less than 1%; Relative peak area 1.23～1.25, RSD is less than 5%), No. 16 peaks (with reference to the peak);
Unimodal area accounts for 2 of the chromatographic peaks of total peak area 5～10%: and No. 10 peaks (relative retention time 0.50～0.52, RSD is less than 1%; Relative peak area 0.44～0.47, RSD is less than 15%), No. 18 peaks (relative retention time 1.00～1.10, RSD is less than 1%; Relative peak area 0.37～0.40, RSD is less than 15%);
Unimodal area accounts for 4 of the chromatographic peaks of total peak area 2～5%: and No. 3 peaks (relative retention time 0.22～0.24, RSD is less than 1%; Relative peak area 0.16～0.18, RSD is less than 5%), No. 4 peaks (relative retention time 0.27～0.29, RSD is less than 1%; Relative peak area 0.19～0.21, RSD is less than 5%), No. 14 peaks (relative retention time 0.68～0.71, RSD is less than 1%; Relative peak area 0.34～0.37, RSD is less than 15%), No. 22 peaks (relative retention time 1.32～1.34, RSD is less than 1%; Relative peak area 0.35～0.37, RSD is less than 10%).
6. the assay method of Colestid efficient liquid-phase chromatograph finger print atlas as claimed in claim 1, it is characterized in that " Chinese medicine fingerprint similarity evaluation systematic study version (2004A) " with the exploitation of different lot number Colestid finger printing data importing Chinese Pharmacopoeia Commission in 2004, the similarity of contrast collection of illustrative plates R of calculating each sample finger printing and generation is all more than 0.9.
7. the assay method of Colestid efficient liquid-phase chromatograph finger print atlas as claimed in claim 1, precision test when it is characterized in that the methodology checking (accurate need testing solution 5～15 μ L that draw, continuous sample introduction 5 times, measure the HPLC collection of illustrative plates), stability test (accurate need testing solution 5～15 μ L that draw, respectively at preparation back 3,6,9,12,15,18, the 24h sample introduction, measure the HPLC collection of illustrative plates) and replica test (get with 5 parts of a collection of medical materials, the preparation need testing solution, the difference sample introduction, measure the HPLC collection of illustrative plates), with 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-glucoside peak (No. 16 peaks) is with reference to the peak, and the RSD value of calculating each total peak relative retention time is less than 2%, and the RSD value of relative peak area is less than 3%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107356684A (en) * | 2017-07-05 | 2017-11-17 | 南京海昌中药集团有限公司 | The detection method of cassia seed finger-print |
| CN114965802A (en) * | 2021-12-14 | 2022-08-30 | 亚宝药业集团股份有限公司 | Quality control method of climacteric syndrome-relieving tablet |
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2009
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107356684A (en) * | 2017-07-05 | 2017-11-17 | 南京海昌中药集团有限公司 | The detection method of cassia seed finger-print |
| CN107356684B (en) * | 2017-07-05 | 2020-03-17 | 南京海昌中药集团有限公司 | Method for detecting fingerprint of cassia seed |
| CN114965802A (en) * | 2021-12-14 | 2022-08-30 | 亚宝药业集团股份有限公司 | Quality control method of climacteric syndrome-relieving tablet |
| CN114965802B (en) * | 2021-12-14 | 2024-04-12 | 亚宝药业集团股份有限公司 | Quality control method of climacteric syndrome relieving tablet |
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