CN105203670A - Establishing method of HPLC (high performance liquid chromatography) fingerprints of loofah sponge, standard fingerprints established with method and application - Google Patents
Establishing method of HPLC (high performance liquid chromatography) fingerprints of loofah sponge, standard fingerprints established with method and application Download PDFInfo
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- CN105203670A CN105203670A CN201510732396.3A CN201510732396A CN105203670A CN 105203670 A CN105203670 A CN 105203670A CN 201510732396 A CN201510732396 A CN 201510732396A CN 105203670 A CN105203670 A CN 105203670A
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Abstract
The invention discloses an establishing method of HPLC (high performance liquid chromatography) fingerprints of loofah sponge, standard fingerprints established with the method and an application and relates to an establishing method of the fingerprints of the loofah sponge, the standard fingerprints established with the method and the application. The method comprises steps as follows: step one, preparation of a solution for test products; step two, preparation of the fingerprints: the solution for test products is injected to a high-performance liquid chromatograph. The fingerprints of the loofah sponge have seven common characteristic peaks, the common characteristic peaks form the fingerprint feature of the loofah sponge, and the fingerprints of the loofah sponge can serve as the standard fingerprints of the loofah sponge. The method has the characteristics of simplicity, convenience, stability, high precision, good reproducibility and easiness in mastering. The fingerprints of the loofah sponge can be applied to authenticity, production place and quality identification and quality control of loofah sponge medicinal materials as the standard fingerprints. The invention applies to the field of medicine.
Description
Technical field
The present invention relates to a kind of method for building up of luffa finger-print and standard finger-print thereof and purposes.
Background technology
Luffa, the i.e. vascular bundle of the dry mature fruit of cucurbitaceous plant sponge gourd Luffacylindrica (L.) Roem..Main containing compositions such as sterol, saponin(e, flavones, phenols, protein, amino acid and organic acids, have dispel the wind, dredging collateral, invigorate blood circulation, effect of lactogenesis, for the contraction of numbness pain, distending pain in the chest and hypochondrium, alactation, acute mastitis such as to swell and ache the disease.Modern study shows, luffa has the effect of Ischemic myocardium, and also achieves good effect in reducing blood lipid, the increase of suppression body weight, anti-inflammatory, antalgic and sedative and antiallergy etc.In quality control, 2010 editions Pharmacopoeias of the People's Republic of China one have recorded luffa medicinal material, but have only carried out powder discriminating.Because the situation such as the place of production, source, collecting season of Chinese medicine is complicated, need to adopt more scientific, rational method to control its quality, this is very necessary to guarantee the safe and effective of clinical application.Finger-print is as extensively being approved at present a kind of technology that Chinese medicine carries out quality control on the whole, and even polycomponent qualitative-and-quantitative method is more obvious compared with one-component for its advantage.The research that there is not yet in current document about luffa finger-print is reported, therefore, for scientificlly and effectively controlling its inherent quality, is necessary the finger-print setting up luffa.
Summary of the invention
The object of this invention is to provide a kind of method for building up of efficient liquid-phase chromatograph finger print atlas of luffa and standard finger-print thereof and purposes.
The method for building up of the efficient liquid-phase chromatograph finger print atlas of luffa of the present invention carries out according to the following steps:
One, the preparation of need testing solution: a, get luffa medicinal material, the mass percentage concentration adding 10 times of quality is 75% ethanol, soak 12h, ultrasonic 30min, filter, collect solid formation A and liquid phase thing A respectively, mass percentage concentration solid formation A being added 10 times of quality is soak 8h in 75% ethanol, ultrasonic 30min, filter, collect liquid phase thing B, then liquid phase thing A and B is mixed, obtain leaching liquor, leaching liquor reduced pressure concentration is obtained medicinal extract;
B, medicinal extract is dissolved with a small amount of distilled water after above first wash 4 column volumes with distilled water in polyamide chromatographic column, then be ethanol elution 4 column volumes of 30% with mass concentration, collect eluent, then reduced pressure concentration eluent is extremely done, and obtains drying solid C;
C, the drying solid C that step b is obtained, be dissolved into methyl alcohol the solution that concentration is 2mg/mL, filter with miillpore filter, filtrate is need testing solution;
Two, the making of finger-print: the need testing solution that step one obtained injects high performance liquid chromatograph take volume ratio as the methyl alcohol of 1:1 and the mixed solution of acetonitrile is A phase, mass percentage concentration be 0.5% acetic acid aqueous solution be that B phase carries out gradient elution; Wherein, high-efficient liquid phase chromatogram condition is: chromatographic column filler ThermoC18, and specification is 250 × 4.6mm, 5 μm; Column temperature is 35 DEG C; Flow velocity 0.8mL/min, determined wavelength 280nm, sample size 20 μ L; Analyze need testing solution with this understanding, obtain the finger-print of luffa.
Three, the determination of standard finger-print: determine 7 common characteristic peaks, with No. 7 peaks for contrast peak, the relative retention time at common characteristic peak is respectively: No. 1 common characteristic peak relative retention time is 0.368 ± 0.003%, No. 2 peak relative retention times are 0.433 ± 0.01%, No. 3 peak relative retention times are 0.462 ± 0.025%, No. 4 peak relative retention times are 0.613 ± 0.016%, No. 5 peak relative retention times are 0.667 ± 0.02%, No. 6 peak relative retention times are 0.881 ± 0.028%, No. 7 peak relative retention times are 1.000, above-mentioned common characteristic peak constitutes the fingerprint characteristic of luffa, can be used as the standard finger-print of luffa.
The purposes of luffa standard finger-print of the present invention refers to luffa finger-print as standard finger-print in luffa quality control.
Beneficial effect of the present invention:
Luffa standard finger-print of the present invention has 7 common characteristic peaks, and these common characteristic peaks constitute the fingerprint characteristic of luffa, can be used as the standard finger-print of luffa.Luffa standard finger-print of the present invention can be used in luffa quality control as standard finger-print after many batch sample checkings, for evaluating and control the quality of luffa medicinal material on the whole, both avoided the one-sidedness judging luffa total quality because only measuring one, two chemical composition, additionally reduce for requisite quality and artificially add contrast composition possibility.The method for building up of the efficient liquid-phase chromatograph finger print atlas of luffa of the present invention have repeatable strong, precision is high and reliable and stable, be easy to the advantage grasped, is applicable to the true and false of luffa medicinal material, the discriminating of the place of production and quality and quality control.
Accompanying drawing explanation
Fig. 1 is for testing the 1 luffa standard finger-print provided; Wherein 1 to 7 is 7 common characteristic peaks of luffa;
Fig. 2 is S1-S10 is 10 batches of luffa medicinal materials fingerprints.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: the method for building up of the efficient liquid-phase chromatograph finger print atlas of present embodiment luffa is carried out according to the following steps:
One, the preparation of need testing solution: a, get luffa medicinal material, the mass percentage concentration adding 10 times of quality is 75% ethanol, soak 12h, ultrasonic 30min, filter, collect solid formation A and liquid phase thing A respectively, mass percentage concentration solid formation A being added 10 times of quality is soak 8h in 75% ethanol, ultrasonic 30min, filter, collect liquid phase thing B, then liquid phase thing A and B is mixed, obtain leaching liquor, leaching liquor reduced pressure concentration is obtained medicinal extract;
B, medicinal extract is dissolved with a small amount of distilled water after above first wash 4 column volumes with distilled water in polyamide chromatographic column, then be ethanol elution 4 column volumes of 30% with mass concentration, collect eluent, then reduced pressure concentration eluent is extremely done, and obtains drying solid C;
C, the drying solid C that step b is obtained, be dissolved into methyl alcohol the solution that concentration is 2mg/mL, filter with miillpore filter, filtrate is need testing solution;
Two, the making of finger-print: the need testing solution that step one obtained injects high performance liquid chromatograph take volume ratio as the methyl alcohol of 1:1 and the mixed solution of acetonitrile is A phase, mass percentage concentration be 0.5% acetic acid aqueous solution be that B phase carries out gradient elution; Wherein, high-efficient liquid phase chromatogram condition is: chromatographic column filler ThermoC18, and specification is 250 × 4.6mm, 5 μm; Column temperature is 35 DEG C; Flow velocity 0.8mL/min, determined wavelength 280nm, sample size 20 μ L; Analyze need testing solution with this understanding, obtain the finger-print of luffa.
Embodiment two: present embodiment and embodiment one unlike: the filtering with microporous membrane in step one is that employing 0.45 μm of miillpore filter filters.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: in step 2, gradient elution order is: 0min → 20min → 50min → 80min, volume ratio is methyl alcohol and the acetonitrile mixed solution 5% → 16% → 25% → 40% of 1:1.Other is identical with embodiment one or two.
Embodiment four: the luffa standard finger-print that present embodiment adopts a kind of method for building up of luffa efficient liquid-phase chromatograph finger print atlas to obtain.
The luffa standard finger-print of present embodiment has 7 common characteristic peaks, and these common characteristic peaks constitute the fingerprint characteristic of luffa, can be used as the standard finger-print of luffa.
Embodiment five: present embodiment and embodiment four unlike: the standard finger-print of luffa has 7 common characteristic peaks, with No. 7 peaks for contrast peak, the relative retention time at common characteristic peak is respectively: No. 1 common characteristic peak relative retention time is 0.368 ± 0.003%, No. 2 peak relative retention times are 0.433 ± 0.01%, No. 3 peak relative retention times are 0.462 ± 0.025%, No. 4 peak relative retention times are 0.613 ± 0.016%, No. 5 peak relative retention times are 0.667 ± 0.02%, No. 6 peak relative retention times are 0.881 ± 0.028%, No. 7 peak relative retention times are 1.000, these 7 common characteristic peaks constitute the fingerprint characteristic of luffa, can be used as the standard finger-print of luffa.Other is identical with embodiment four.
Embodiment six: the purposes of present embodiment luffa standard finger-print refers to luffa finger-print as standard finger-print in luffa quality control.
The luffa standard finger-print of present embodiment can be used in luffa quality control as standard finger-print after many batch sample checkings, for evaluating and control the quality of luffa medicinal material on the whole, both avoided the one-sidedness judging luffa total quality because only measuring one, two chemical composition, additionally reduce for requisite quality and artificially add contrast composition possibility.
By following verification experimental verification beneficial effect of the present invention:
Test 1:
1, test method: the method for building up of the efficient liquid-phase chromatograph finger print atlas of this test luffa is carried out according to the following steps:
One, the preparation of need testing solution: a, get luffa medicinal material, the mass percentage concentration adding 10 times of quality is 75% ethanol, soak 12h, ultrasonic 30min, filter, collect solid formation A and liquid phase thing A respectively, mass percentage concentration solid formation A being added 10 times of quality is soak 8h in 75% ethanol, ultrasonic 30min, filter, collect liquid phase thing B, then liquid phase thing A and B is mixed, obtain leaching liquor, leaching liquor reduced pressure concentration is obtained medicinal extract;
B, medicinal extract is dissolved with a small amount of distilled water after above first wash 4 column volumes with distilled water in polyamide chromatographic column, then be ethanol elution 4 column volumes of 30% with mass concentration, collect eluent, then reduced pressure concentration eluent is extremely done, and obtains drying solid C;
C, the drying solid C that step b is obtained, be dissolved into methyl alcohol the solution that concentration is 2mg/mL, filter with miillpore filter, filtrate is need testing solution;
Two, the making of finger-print: the need testing solution that step one obtained injects high performance liquid chromatograph take volume ratio as the methyl alcohol of 1:1 and the mixed solution of acetonitrile is A phase, mass percentage concentration be 0.5% acetic acid aqueous solution be that B phase carries out gradient elution; Wherein, high-efficient liquid phase chromatogram condition is: 1, chromatographic column filler ThermoC18, and specification is 250 × 4.6mm, 5 μm; Column temperature is 35 DEG C; Adopt gradient elution mode 0min → 20min → 50min → 80min, volume ratio is methyl alcohol and the acetonitrile mixed solution 5% → 16% → 25% → 40% of 1:1; Flow velocity 0.8mL/min, determined wavelength 280nm, sample size 20 μ L;
2, test apparatus: HITACHIL-2000 high performance liquid chromatograph; HITACHIL-2400 UV-detector; AT-130 chromatographic column column oven; HITACHID-2000 chromatographic work station.
3, test material: 10 batches of luffa medicinal materials are from Hunan, Shandong, Anhui, Zhejiang, Guangxi, Shanxi, Jiangsu and other places.
According to the method for building up of the efficient liquid-phase chromatograph finger print atlas of the luffa of this test, efficient liquid-phase chromatograph finger print atlas is established to 10 batches of luffa medicinal materials, the spectrogram obtained imports chromatographic fingerprints of Chinese materia medica Similarity Measure software (the Pharmacopoeia of People's Republic of China council, version in 2004), determine 7 common characteristic peaks, with No. 7 peaks for contrast peak, the relative retention time at common characteristic peak is respectively: No. 1 common characteristic peak relative retention time is 0.368 ± 0.003%, No. 2 peak relative retention times are 0.433 ± 0.01%, No. 3 peak relative retention times are 0.462 ± 0.025%, No. 4 peak relative retention times are 0.613 ± 0.016%, No. 5 peak relative retention times are 0.667 ± 0.02%, No. 6 peak relative retention times are 0.881 ± 0.028%, No. 7 peak relative retention times are 1.000, above-mentioned common characteristic peak constitutes the fingerprint characteristic of luffa, can be used as the standard finger-print of luffa.
The standard finger-print of the luffa that this test obtains as shown in Figure 1.As seen from Figure 1, clearly can be obtained the standard finger-print of the luffa with 7 common characteristic peaks by this method, the quality for overall evaluation luffa provides good foundation.
4, methodological study
4.1 method reappearance is tested
Get with a collection of luffa medicinal material 6 parts, need testing solution is prepared according to the preparation method of luffa need testing solution in test method, carry out determining fingerprint pattern, respectively the relative retention time at total peak and relative peak area are added up, result is as shown in table 1, RSD% is all no more than 3%, shows method reappearance of the present invention good.
4.2 finger-print precision tests
The need testing solution of access method reappearance test is a, continuous sample introduction 5 times, and add up the relative retention time at total peak and relative peak area respectively, RSD% was all no more than for 3% (as table 2), and it is good that result shows method precision of the present invention.
4.3 finger-print stability tests
The need testing solution of access method reappearance test is a, carry out determining fingerprint pattern, investigate the stability in need testing solution 48 hours, respectively the relative retention time at total peak and relative peak area are added up, RSD% was all no more than for 3% (as table 3), and result display need testing solution is stable in 48 hours.
Above test findings display, this assay method is reliable and stable, and finger-print is relatively stable.
Table 1 reproducible test results (n=6)
Table 2 Precision test result (n=5)
Table 3 stability test result (n=5)
Claims (6)
1. a method for building up for the efficient liquid-phase chromatograph finger print atlas of luffa, is characterized in that the method is carried out according to the following steps:
One, the preparation of need testing solution: a, get luffa medicinal material, the mass percentage concentration adding 10 times of quality is 75% ethanol, soak 12h, ultrasonic 30min, filter, collect solid formation A and liquid phase thing A respectively, mass percentage concentration solid formation A being added 10 times of quality is soak 8h in 75% ethanol, ultrasonic 30min, filter, collect liquid phase thing B, then liquid phase thing A and B is mixed, obtain leaching liquor, leaching liquor reduced pressure concentration is obtained medicinal extract;
B, medicinal extract is dissolved with distilled water after upper in polyamide chromatographic column, first wash 4 column volumes with distilled water, then be ethanol elution 4 column volumes of 30% with mass concentration, collect eluent, then reduced pressure concentration eluent is extremely done, and obtains drying solid C;
C, the drying solid C that step b is obtained, be dissolved into methyl alcohol the solution that concentration is 2mg/mL, filter with miillpore filter, filtrate is need testing solution;
Two, the making of finger-print: the need testing solution that step one obtained injects high performance liquid chromatograph take volume ratio as the methyl alcohol of 1:1 and the mixed solution of acetonitrile is A phase, mass percentage concentration be 0.5% acetic acid aqueous solution be that B phase carries out gradient elution; Wherein, high-efficient liquid phase chromatogram condition is: chromatographic column filler ThermoC18, and specification is 250 × 4.6mm, 5 μm; Column temperature is 35 DEG C; Flow velocity 0.8mL/min, determined wavelength 280nm, sample size 20 μ L; Analyze need testing solution with this understanding, obtain the finger-print of luffa.
2. the method for building up of the efficient liquid-phase chromatograph finger print atlas of a kind of luffa according to claim 1, is characterized in that gradient elution order is: the filtering with microporous membrane in step one is that employing 0.45 μm of miillpore filter filters.
3. the method for building up of the efficient liquid-phase chromatograph finger print atlas of a kind of luffa according to claim 1, it is characterized in that in step 2, gradient elution order is: 0min → 20min → 50min → 80min, volume ratio is methyl alcohol and the acetonitrile mixed solution 5% → 16% → 25% → 40% of 1:1.
4. adopt the luffa standard finger-print that the method for building up of the efficient liquid-phase chromatograph finger print atlas of a kind of luffa according to claim 1 obtains.
5. luffa standard finger-print according to claim 4, it is characterized in that the finger-print of luffa has 7 common characteristic peaks, with No. 7 peaks for contrast peak, the relative retention time at common characteristic peak is respectively: No. 1 common characteristic peak relative retention time is 0.368 ± 0.003%, No. 2 peak relative retention times are 0.433 ± 0.01%, No. 3 peak relative retention times are 0.462 ± 0.025%, No. 4 peak relative retention times are 0.613 ± 0.016%, No. 5 peak relative retention times are 0.667 ± 0.02%, No. 6 peak relative retention times are 0.881 ± 0.028%, No. 7 peak relative retention times are 1.000, these 7 common characteristic peaks constitute the fingerprint characteristic of luffa, can be used as the standard finger-print of luffa.
6. the purposes of luffa standard finger-print, is characterized in that luffa standard finger-print as standard finger-print in luffa quality control.
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