CN104569275A - Method for simultaneously measuring concentrations of monomer components including ursolic acid, schizandrin a, schizandrin b and schizandrin c - Google Patents
Method for simultaneously measuring concentrations of monomer components including ursolic acid, schizandrin a, schizandrin b and schizandrin c Download PDFInfo
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Abstract
The invention discloses a method for simultaneously measuring the concentrations of monomer components including ursolic acid, schizandrin a, schizandrin b and schizandrin c, belonging to material analysis by using a chromatography. The method disclosed by the invention comprises the following steps: respectively preparing a mixed sample of dogwood and schisandra chinensis and a negative control solution of a sample to be measured, and, after pre-processing, carrying out preparation of a working curve and chromatographic separation and content determination of the four monomer components under the conditions as follows: a mobile phase is the mixture of acetonitrile and 0.1% phosphoric acid aqueous solution with the ratio of 67 to 33; the volume flow rate is 0.8-1.2 mL/min; the ultraviolet detection wavelength is 190-220 nm; and the column temperature is 25-40 DEG C. Simultaneous concentration detection and complete separation of the four monomer components including ursolic acid, schizandrin a, schizandrin b and schizandrin c are realized within a relatively short time under same wavelength chromatographic experimental conditions; the method disclosed by the invention has the advantages of being steady in base line, symmetrical and attractive in peak pattern, simple, convenient, rapid, high in separation degree and sensitivity, good in repeatability, accurate and reliable in data and high in recovery; and therefore, a good quality control detection method is provided.
Description
Technical field
The present invention relates to chromatograph Material Field, specifically a kind of method of Simultaneously test ursolic acid and the fruit of Chinese magnoliavine first and second C prime monomer component concentration.
Background technology
Traditional Chinese medicine especially natural traditional Chinese medicine multiply the mankind in several thousand, survive, develop in play an important role, and the fruit of Chinese magnoliavine, the fruit of medicinal cornel are exactly the medicinal material of this wherein outbalance.The fruit of Chinese magnoliavine is perennial fallen leaves liana, and belong to Magnoliaceae, this medicine is multiple functional, and the five tastes all have, therefore has the title of the fruit of Chinese magnoliavine.In Chinese medicinal material, the five tastes have concurrently and belong to exclusive in fact, and it has unique curative effect to the deficiency of Yin and the deficiency of yang.The fruit of Chinese magnoliavine has nourshing kidney of astringing the lung, effect of the arrest sweating that promotes the production of body fluid, puckery smart antidiarrheal, antitoxic heart-soothing and sedative.The fruit of Chinese magnoliavine is mainly containing principal ingredients such as lignanoid, volatile oil, organic acid, triterpene, sequiterpenes, and wherein Lignanoids compounds mainly comprises schizandrin A, deoxyschizandrin and schisandrin C etc.Modern pharmacology shows, fruit of Chinese magnoliavine first, second, C prime have many pharmacologically actives, and as having sedation to central nervous system, too high to chronic hepatitis, neurasthenia, gastric acidity, the diseases such as ulcer have good clinical efficacy.The fruit of medicinal cornel is deciduous tree or dungarunga, and drying and ripening pulp is used as medicine.The fruit of medicinal cornel has tonifying the liver and kidney, restrains astringent or styptic treatment for spontaneous sweating effect.The fruit of medicinal cornel is mainly containing multiple elements such as loganin, cornin, the new glycosides of the fruit of medicinal cornel, ursolic acid, oleanolic acids.Modern pharmacology shows, ursolic acid has reduction blood sugar, the effect such as anti-ageing and immunological regulation.As can be seen here, ursolic acid and fruit of Chinese magnoliavine first, second, C prime are that the Chinese medicine fruit of medicinal cornel and the fruit of Chinese magnoliavine play the most key active monomer component of pharmacological action.Therefore, the Quality Control detection method of detection fruit of Chinese magnoliavine first, second, C prime and ursolic acid is simultaneously found to ensureing that the quality of the pharmaceutical preparations is vital.
In prior art, when detecting fruit of Chinese magnoliavine first, second, C prime by reversed-phased high performace liquid chromatographic, adopt linear gradient elution method more simultaneously, selection 250nm is absorbing wavelength, owing to will convert the ratio of mobile phase in experimentation, can cause baseline fluctuation, sensitivity decrease, affects the accuracy of experimental result; And majority goes out peak after 30min, cause experimental period long.
Summary of the invention
The present invention is exactly to overcome in prior art, linear gradient elution method causes baseline fluctuation when detecting fruit of Chinese magnoliavine first, second, C prime simultaneously, sensitivity decrease, and simultaneously can not detect the shortcoming of ursolic acid and fruit of Chinese magnoliavine first, second, C prime four kinds of active monomer components, and the method for a kind of isocratic elution method Simultaneously test ursolic acid provided and the fruit of Chinese magnoliavine first and second C prime monomer component concentration.
The present invention realizes according to following technical scheme.
A method for Simultaneously test ursolic acid and the fruit of Chinese magnoliavine first and second C prime monomer component concentration, comprises the following steps:
A. the pre-service of sample
The fruit of Chinese magnoliavine, be dried to constant weight containing the ursolic acid medicinal material fruit of medicinal cornel, cross 40 mesh sieves after pulverizing, take containing the ursolic acid medicinal material fruit of medicinal cornel 10 parts by ratio of weight and the number of copies respectively, 1 part, the fruit of Chinese magnoliavine, after mixing, add 10 times amount absolute ethyl alcohols; Ultrasound wave extracts and suction filtration, and filtrate crosses 0.22 μm of miillpore filter, sample size 3-20 μ L;
Testing sample lacks the preparation containing ursolic acid medicinal material fruit of medicinal cornel negative control solution: essence claims 1 part of Chinese Magnolivine Fruit, preparation, filter, sample size is the same;
Testing sample lacks the preparation of fruit of Chinese magnoliavine negative control solution: essence claims 10 parts containing ursolic acid medicinal material Asiatic Cornelian Cherry Fruit, preparation, filter, sample size is the same;
B. high performance liquid chromatography operating conditions
Agilent 1260 type high performance liquid chromatograph; Chromatographic column: 150 × 46 mm, 5 μm, ZORBAX SB-C18; Mobile phase is acetonitrile 67-70%
:0.1% phosphate aqueous solution 33-30%, volumetric flow rate is 0.8-1.2 mL/min; UV detect wavelength is 190-220 nm; Column temperature 25-40 DEG C;
The condition that ultrasound wave extracts is 250W, 40KHz, and 20 DEG C, ultrasonic time is 30min;
C. the preparation of working curve
Precision takes ursolic acid reference substance 1.36 mg, A prime reference substance 1.0 mg, deoxyschizandrin reference substance 1.36 mg, schisandrin C reference substance 0.82 mg respectively, be made into the absolute ethyl alcohol mixing reference substance solution of 1mL, and carry out doubling dilution, obtain 8 mass concentrations of four kinds of monomer mixing reference substance dilute solutions altogether, get rear 7 mass concentrations and the peak area of sample introduction mensuration and corresponding concentration drawing standard curve; Each mass concentration liquid crosses 0.22 μm of miillpore filter respectively, and sample introduction 10 μ L carries out stratographic analysis, with peak area
ato concentration
ccarry out linear regression, obtain four kinds of monomer component working curves simultaneously;
D. the chromatographic resolution of four kinds of monomer components and the mensuration of content
Upper machine mensuration will be carried out through the pretreated fruit of Chinese magnoliavine with containing ursolic acid medicinal material fruit of medicinal cornel sample, four kinds of monomer components carry out chromatographic resolution, and are calculated the content of four kinds of monomer components respectively by corresponding working curve according to peak area corresponding to traditional Chinese medicine monomer composition each in testing sample.
The invention has the beneficial effects as follows:
The present invention (25min) can utilize isocratic elution method in relative short time, under Same Wavelength chromatography experiment condition, detects simultaneously and is separated traditional Chinese medicine monomer composition-ursolic acid and fruit of Chinese magnoliavine first, second, the C prime with valuable pharmacological activity completely.Use the concentration of method Simultaneously test of the present invention four kinds of monomer components, baseline is steady, and peak type symmetry is attractive in appearance, fast easy, and degree of separation is high, highly sensitive, reproducible, and accurately and reliably, the recovery is high for data, provides a kind of good Quality Control detection means.
Accompanying drawing explanation
Fig. 1 is control sample high-efficient liquid phase chromatogram of the present invention;
Fig. 2 is testing sample high-efficient liquid phase chromatogram of the present invention;
Fig. 3 is the negative control solution high-efficient liquid phase chromatogram that testing sample of the present invention lacks the fruit of Chinese magnoliavine;
Fig. 4 is the negative control solution high-efficient liquid phase chromatogram that testing sample of the present invention lacks the fruit of medicinal cornel.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.
1. instrument and material
2.1 instrument
Agilent 1260 type high performance liquid chromatograph, comprises quaternary pump, G1311C, automatic sampler, G1329B, VWD detecting device, G1314F, chromatographic work station, Anjelen Sci. & Tech. Inc;
AE240 precise electronic analytical balance, plum Teller-Shanghai holder benefit instrument;
Superpure water machine, French MILLIPORE;
Universalpulverizer, Beijing Zhong Xing great achievement Instrument Ltd. manufactures;
Supersonic extractors, Xin Yi biotech inc, Ningbo;
Electric drying oven with forced convection, Tianjin three hydroscience Instrument Ltd..
2.2 material
Fruit of Chinese magnoliavine first, second, C prime reference substance, Nat'l Pharmaceutical & Biological Products Control Institute, massfraction is no less than 99.9%, lot number 20130306;
Ursolic acid, Nat'l Pharmaceutical & Biological Products Control Institute, massfraction is no less than 99.9%, lot number 20130406;
Acetonitrile (chromatographically pure), German Merk company;
Phosphoric acid (chromatographically pure), Tianjin recovery fine chemistry industry research institute;
Experimental water is secondarily purified water, and Tianjin City No.1 Central Hospital pharmaceutical factory provides.
2. experimental technique and result
The pre-service of 2.1 samples
The fruit of Chinese magnoliavine, be dried to constant weight containing at the ursolic acid medicinal material fruit of medicinal cornel 60 DEG C, cross 40 mesh sieves after pulverizing, precision takes containing ursolic acid medicinal material fruit of medicinal cornel 1g respectively, and fruit of Chinese magnoliavine 0.1g, pours into the powder of mixing in 25ml conical flask, adds 1mL absolute ethyl alcohol.At 250W, 40KHz, under 20 DEG C of experiment conditions, ultrasonic extraction 30min, the ethanolic solution that suction filtration extracts, filtrate crosses 0.22 μm of miillpore filter, sample introduction 10 μ L.
Testing sample lacks the preparation containing ursolic acid medicinal material fruit of medicinal cornel negative control solution: essence claims Chinese Magnolivine Fruit 0.1g, pours in conical flask, add 1mL absolute ethyl alcohol by the powder of mixing; At 250W, 40KHz, under 20 DEG C of experiment conditions, ultrasonic extraction 30min, the ethanolic solution that suction filtration extracts, filtrate crosses 0.22 μm of miillpore filter, sample introduction 10 μ L.
Testing sample lacks the preparation of fruit of Chinese magnoliavine negative control solution: essence claims, containing ursolic acid medicinal material Asiatic Cornelian Cherry Fruit 1g, to pour in conical flask, add 10mL absolute ethyl alcohol by the powder of mixing; At 250W, 40KHz, under 20 DEG C of experiment conditions, ultrasonic extraction 30min, the ethanolic solution that suction filtration extracts, filtrate crosses 0.22 μm of miillpore filter, sample introduction 10 μ L.
2.2 chromatographic condition
Agilent 1260 type high performance liquid chromatograph; Chromatographic column: ZORBAX SB-C
18(150 × 46 mm, 5 μm) chromatographic column.Mobile phase is acetonitrile: 0.1% phosphate aqueous solution=67:33, volumetric flow rate 1.0 mL/min; UV detect wavelength is 210 nm; Column temperature 30 DEG C; Sample size 10 μ L.
The preparation of 2.3 working curves
Precision takes ursolic acid reference substance 1.36 mg, A prime reference substance 1.0 mg, deoxyschizandrin reference substance 1.36 mg, schisandrin C reference substance 0.82 mg respectively, be made into the absolute ethyl alcohol mixing reference substance solution of 1mL, and carry out doubling dilution, obtain 8 mass concentrations of four kinds of monomer mixing reference substance dilute solutions, get rear 7 mass concentrations and the peak area that measures of sample introduction and corresponding concentration obtain the working curve of four kinds of monomer components simultaneously.
2.3.1 ursolic acid working curve
In each 8 mass concentrations of the four kinds of monomer mixing reference substance dilute solutions obtained, the mass concentration obtaining ursolic acid dilute solution is 680,340,170,85,42.5,21.25,10.625,5.313 mg/L; Get rear 7 mass concentrations and the peak area of sample introduction mensuration and corresponding concentration drawing standard curve; Each mass concentration liquid crosses 0.22 μm of miillpore filter respectively, and sample introduction 10 μ L carries out stratographic analysis; With peak area
ato concentration
c(mg/L) carry out linear regression, obtain ursolic acid working curve: A=6.135C+18.700, r=0.9995; Ursolic acid is good linear relationship with peak area between mass concentration 340 ~ 5.313 mg/L; According to signal to noise ratio (S/N ratio) 3/1, ursolic acid lowest detection mass concentration is 0.025 mg/L.
2.3.2 schizandrin A working curve
In each 8 mass concentrations of the four kinds of monomer mixing reference substance dilute solutions obtained, the mass concentration obtaining schizandrin A dilute solution is 500,250,125,62.5,31.25,15.625,7.812,3.906 mg/L; Get rear 7 mass concentrations and the peak area of sample introduction mensuration and corresponding concentration drawing standard curve; Each mass concentration liquid crosses 0.22 μm of miillpore filter respectively, and sample introduction 10 μ L carries out stratographic analysis; With peak area
ato concentration
c(mg/L) carry out linear regression, obtain schizandrin A working curve: A=79.196C+196.449, r=0.9994; Schizandrin A is good linear relationship with peak area between mass concentration 250 ~ 3.906 mg/L; According to signal to noise ratio (S/N ratio) 3/1, the lowest detection mass concentration of schizandrin A is 0.016 mg/L.
2.3.3 deoxyschizandrin working curve
In each 8 mass concentrations of the four kinds of monomer mixing reference substance dilute solutions obtained, the mass concentration obtaining deoxyschizandrin dilute solution is 680,340,170,85,42.5,21.25,10.625,5.313 mg/L; Get rear 7 mass concentrations and the peak area that records of sample introduction and corresponding concentration drawing standard curve; Each mass concentration liquid crosses 0.22 μm of miillpore filter respectively, and sample introduction 10 μ L carries out stratographic analysis; With peak area
ato concentration
c(mg/L) carry out linear regression, obtain deoxyschizandrin working curve: A=22.085C+66.829, r=0.9995; Deoxyschizandrin is good linear relationship with peak area between mass concentration 340 ~ 5.313 mg/L; According to signal to noise ratio (S/N ratio) 3/1, the lowest detection mass concentration of deoxyschizandrin is 0.019 mg/L.
2.3.4 schisandrin C working curve
In each 8 mass concentrations of the four kinds of monomer mixing reference substance dilute solutions obtained, the mass concentration obtaining schisandrin C dilute solution is 410,205,102.5,51.25,25.625,12.810,6.450,3.225 mg/L; Get rear 7 mass concentrations and the peak area that records of sample introduction and corresponding concentration drawing standard curve; Each mass concentration liquid crosses 0.22 μm of miillpore filter respectively, and sample introduction 10 μ L carries out stratographic analysis; With peak area
ato concentration
c(mg/L) carry out linear regression, obtain schisandrin C working curve: A=23.106C+43.569, r=0.9995; Schisandrin C is good linear relationship with peak area between mass concentration 205 ~ 3.225 mg/L; According to signal to noise ratio (S/N ratio) 3/1, the lowest detection mass concentration of schisandrin C is 0.020 mg/L.
2.4 chromatographic resolution
Respectively chromatographic resolution is carried out to the ursolic acid in sample to be tested and fruit of Chinese magnoliavine first, second, C prime, the results are shown in Figure 1, in 2(figure: 1: schizandrin A; 2: deoxyschizandrin; 3: schisandrin C; 4: ursolic acid).Visible, the separation of each component all can reach baseline separation, and peak type is symmetrical, and degree of separation is good, and disturbs without obvious impurity peaks.The retention time of ursolic acid is 23.003 min; The retention time of schizandrin A is 10.401 min; The retention time of deoxyschizandrin is 13.329 min; The retention time of schisandrin C is 15.388 min.
Do the negative control experiment that sample to be tested lacks the fruit of Chinese magnoliavine and the fruit of medicinal cornel respectively respectively, the results are shown in Figure 3 and 4.Visible, Fig. 3 does not detect the chromatographic peak of these three kinds of monomer components in fruit of Chinese magnoliavine first, second, the corresponding retention time of C prime; Fig. 4 does not detect its chromatographic peak in the corresponding retention time of ursolic acid.Illustrate detect this four kinds of monomer components time do not have Interference Peaks to occur.
2.5 precision tests (RSD)
To the same mixing contrast solution that schizandrin A concentration is 15.620 mg/L, deoxyschizandrin concentration is 21.25 mg/L, schisandrin C concentration is 25.625 mg/L, ursolic acid concentration is 21.25 mg/L, continuous sample introduction 5 times, record the chromatographic peak area numerical value of corresponding monomer component respectively, and through statistical procedures, measure that ursolic acid RSD is 1.86%, schizandrin A RSD is 1.76%, deoxyschizandrin RSD is 1.69%, schisandrin C RSD is 1.80%(n=5).
2.6 replica test
Prepare 6 parts of product to be tested solution according to the preparation method of above-mentioned product to be tested simultaneously, sample introduction 1 time respectively, record the chromatographic peak area numerical value of corresponding monomer component, and through statistical procedures method, ursolic acid RSD is 1.56%, schizandrin A RSD is 1.77%, deoxyschizandrin RSD is 1.66%, schisandrin C RSD is 1.49%(n=6).
2.7 mean sample recovery rate tests
In 0.9 mL sample to be tested solution, (detecting ursolic acid mass concentration is 1.635 mg/L; Schizandrin A is 1.361mg/L; Deoxyschizandrin is 9.238mg/L; Schisandrin C is 0.953mg/L) add 0.1 mL mixing reference substance solution respectively, ursolic acid mass concentration is respectively 10.625,21.25,42.5 mg/L; Schizandrin A mass concentration is respectively 7.812,15.620,31.25 mg/L; Deoxyschizandrin mass concentration is respectively 10.625,21.25,42.5 mg/L; Schisandrin C mass concentration is respectively 6.406,12.813,25,625 mg/L.Sample introduction records its mass concentration, calculates its recovery, and result ursolic acid average recovery rate is 101.16%, RSD is 1.36%; Schizandrin A average recovery rate is 100.79%, RSD is 1.41%; Deoxyschizandrin average recovery rate is 101.09%, RSD is 1.49%; Schisandrin C average recovery rate is 101.26%, RSD is 1.31%.
2.8 stability test
Same sample to be tested is measured relevant corresponding chromatogram value at 0,4,8,12,24,48 h respectively.The RSD of result ursolic acid is 1.56%; The RSD of schizandrin A is 1.61%; The RSD of deoxyschizandrin is 1.39%; The RSD of schisandrin C is 1.60%.In display sample to be tested 48 h, sample is stablized.
The mensuration of 2.9 sample to be tested content
Record the amount of ursolic acid and fruit of Chinese magnoliavine first, second in 5 samples to be tested, C prime respectively, the results are shown in Table 1.
Ursolic acid and the fruit of Chinese magnoliavine first and second C prime assay (mg/g) in table 1. sample to be tested
In sum, application the present invention (25min) can utilize isocratic elution method in relative short time, under Same Wavelength chromatography experiment condition, detect simultaneously and be separated traditional Chinese medicine monomer composition-ursolic acid and fruit of Chinese magnoliavine first, second, the C prime with valuable pharmacological activity completely.Use method of the present invention to measure the concentration of four kinds of monomer components, baseline is steady, and peak type symmetry is attractive in appearance, fast easy, and degree of separation is high, highly sensitive, reproducible, and accurately and reliably, the recovery is high for data, provides a kind of good Quality Control detection means.
Claims (5)
1. a method for Simultaneously test ursolic acid and the fruit of Chinese magnoliavine first and second C prime monomer component concentration, is characterized in that: comprise the following steps:
A. the pre-service of sample
The fruit of Chinese magnoliavine, be dried to constant weight containing the ursolic acid medicinal material fruit of medicinal cornel, cross 40 mesh sieves after pulverizing, take containing the ursolic acid medicinal material fruit of medicinal cornel 10 parts by ratio of weight and the number of copies respectively, 1 part, the fruit of Chinese magnoliavine, after mixing, add 10 times amount absolute ethyl alcohols; Ultrasound wave extracts and suction filtration, and filtrate crosses 0.22 μm of miillpore filter, sample size 3-20 μ l;
Testing sample lacks the preparation containing ursolic acid medicinal material fruit of medicinal cornel negative control solution: essence claims 1 part of Chinese Magnolivine Fruit, preparation, filter, sample size is the same;
Testing sample lacks the preparation of fruit of Chinese magnoliavine negative control solution: essence claims 10 parts containing ursolic acid medicinal material Asiatic Cornelian Cherry Fruit, preparation, filter, sample size is the same;
B. high performance liquid chromatography operating conditions
Agilent 1260 type high performance liquid chromatograph; Chromatographic column: 150 × 46 mm, 5 μm, ZORBAX SB-C18; Mobile phase is acetonitrile 67-70%
:0.1% phosphate aqueous solution 33-30%, volumetric flow rate is 0.8-1.2 mL/min; UV detect wavelength is 190-220 nm; Column temperature 25-40 DEG C;
The condition that ultrasound wave extracts is 250W, 40KHz, and 20 DEG C, ultrasonic time is 30min;
C. the preparation of working curve
Precision takes ursolic acid reference substance 1.36 mg, A prime reference substance 1.0 mg, deoxyschizandrin reference substance 1.36 mg, schisandrin C reference substance 0.82 mg respectively, be made into the absolute ethyl alcohol mixing reference substance solution of 1mL, and carry out doubling dilution, obtain 8 mass concentrations of four kinds of monomer mixing reference substance dilute solutions altogether, get peak area and the corresponding concentration drawing standard curve of rear 7 mass concentration sample introductions mensuration; Each mass concentration liquid crosses 0.22 μm of miillpore filter respectively, and sample introduction 10 μ L carries out stratographic analysis, with peak area
ato concentration
ccarry out linear regression, obtain four kinds of monomer component working curves simultaneously;
D. the chromatographic resolution of four kinds of monomer components and the mensuration of content
Upper machine mensuration will be carried out through the pretreated fruit of Chinese magnoliavine with containing ursolic acid medicinal material fruit of medicinal cornel sample, four kinds of monomer components carry out chromatographic resolution, and are calculated the content of four kinds of monomer components respectively by corresponding working curve according to peak area corresponding to traditional Chinese medicine monomer composition each in testing sample.
2. the method for a kind of Simultaneously test ursolic acid according to claim 1 and the fruit of Chinese magnoliavine first and second C prime monomer component concentration, it is characterized in that: in four kinds of monomer mixing reference substance dilute solutions, 8 mass concentrations obtaining ursolic acid dilute solution are respectively 680,340,170,85,42.5,21.25,10.625,5.313 mg/L; Get rear 7 mass concentrations and sample introduction measure peak area and corresponding concentration obtain ursolic acid working curve: A=6.135C+18.700, r=0.9995;
Ursolic acid is good linear relationship with peak area between mass concentration 340 ~ 5.313 mg/L; According to signal to noise ratio (S/N ratio) 3/1, ursolic acid lowest detection mass concentration is 0.025 mg/L.
3. the method for a kind of Simultaneously test ursolic acid according to claim 1 and the fruit of Chinese magnoliavine first and second C prime monomer component concentration, it is characterized in that: in four kinds of monomer mixing reference substance dilute solutions, 8 mass concentrations obtaining schizandrin A dilute solution are respectively 500,250,125,62.5,31.25,15.625,7.812,3.906 mg/L; Get rear 7 mass concentrations and sample introduction measure peak area and corresponding concentration obtain schizandrin A working curve: A=79.196C+196.449, r=0.9994;
Schizandrin A is good linear relationship with peak area between mass concentration 250 ~ 3.906 mg/L; According to signal to noise ratio (S/N ratio) 3/1, the lowest detection mass concentration of schizandrin A is 0.016 mg/L.
4. the method for ursolic acid and the fruit of Chinese magnoliavine first and second C prime in a kind of Simultaneously test fruit of medicinal cornel according to claim 1, it is characterized in that: in four kinds of monomer mixing reference substance dilute solutions, 8 mass concentrations obtaining deoxyschizandrin dilute solution are respectively 680,340,170,85,42.5,21.25,10.625,5.313 mg/L; Get rear 7 mass concentrations and sample introduction measure peak area and corresponding concentration obtain deoxyschizandrin working curve: A=22.085C+66.829, r=0.9995;
Deoxyschizandrin is good linear relationship with peak area between mass concentration 340 ~ 5.313 mg/L; According to signal to noise ratio (S/N ratio) 3/1, the lowest detection mass concentration of deoxyschizandrin is 0.019 mg/L.
5. the method for ursolic acid and the fruit of Chinese magnoliavine first and second C prime in a kind of Simultaneously test fruit of medicinal cornel according to claim 1, is characterized in that: in four kinds of monomer mixing reference substance dilute solutions
,8 mass concentrations obtaining schisandrin C dilute solution are respectively 410,205,102.5,51.25,25.625,12.810,6.450,3.225 mg/L; Get rear 7 mass concentrations and sample introduction measure peak area and corresponding concentration obtain schisandrin C working curve: A=23.106C+43.569, r=0.9995;
Schisandrin C is good linear relationship with peak area between mass concentration 205 ~ 3.225 mg/L; According to signal to noise ratio (S/N ratio) 3/1, the lowest detection mass concentration of schisandrin C is 0.020 mg/L.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030026854A1 (en) * | 2001-04-04 | 2003-02-06 | Xinxian Zhao | Plant drug for treatment of liver disease |
| CN1836717A (en) * | 2004-12-13 | 2006-09-27 | 贵阳云岩西创药物科技开发有限公司 | Quality controlling method for pulse restoring injection |
| CN1911393A (en) * | 2005-08-12 | 2007-02-14 | 北京联合西创药物科技有限公司 | Injection contg. traditional Chinese medicine, and its quality control method |
| CN101709059A (en) * | 2009-12-09 | 2010-05-19 | 北京博远欣绿科技有限公司 | Chinese magnoliavine fruit monomer composition separation preparation method |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030026854A1 (en) * | 2001-04-04 | 2003-02-06 | Xinxian Zhao | Plant drug for treatment of liver disease |
| CN1836717A (en) * | 2004-12-13 | 2006-09-27 | 贵阳云岩西创药物科技开发有限公司 | Quality controlling method for pulse restoring injection |
| CN1911393A (en) * | 2005-08-12 | 2007-02-14 | 北京联合西创药物科技有限公司 | Injection contg. traditional Chinese medicine, and its quality control method |
| CN101709059A (en) * | 2009-12-09 | 2010-05-19 | 北京博远欣绿科技有限公司 | Chinese magnoliavine fruit monomer composition separation preparation method |
Non-Patent Citations (2)
| Title |
|---|
| Y. H. CHOI等: "Optimum SFE Condition for Lignans of Schisandra chinensis Fruits", 《CHROMATOGRAPHIA》 * |
| 洪海等: "高效液相色谱法测定强肝消脂胶囊中熊果酸的含量", 《中国医药指南》 * |
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