CN100573140C - Schisandra raw material fingerprint quality determining method in the body resistance-strengthening stasis-eliminating plant drug - Google Patents

Schisandra raw material fingerprint quality determining method in the body resistance-strengthening stasis-eliminating plant drug Download PDF

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CN100573140C
CN100573140C CNB2007100403318A CN200710040331A CN100573140C CN 100573140 C CN100573140 C CN 100573140C CN B2007100403318 A CNB2007100403318 A CN B2007100403318A CN 200710040331 A CN200710040331 A CN 200710040331A CN 100573140 C CN100573140 C CN 100573140C
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胡坪
潘一峰
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Shanghai Baiyang Pharmaceutical Co ltd
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SHANGHAI MODERN CHINESE TRADITIONAL MEDICINE TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

The present invention relates to schisandra raw material fingerprint quality determining method in the body resistance-strengthening stasis-eliminating plant drug, comprising: (1) gets the 0.5g fruit of Chinese magnoliavine, and ultrasonic Extraction 50min filters; (2) gradient elution moving phase: chromatographic column is Eclipse; 0-40min, 60-20%A, 40-80%B; Flow velocity 0.8-1.2ml/min; Wavelength 210-280nm, column temperature 20-40 ℃; Sample size 10-20 μ l; (3) foundation of standard finger-print: No. 1 peak schizandrin, No. 3 peak wuweizi alcohol Bs, No. 4 peak Ge Mixin N/ isomeride, No. 6 peak schizandrin As, No. 7 peaks and No. 8 peak Ge Mixin N/ isomeride, No. 9 peak deoxyschizandrins; (4) quality control of finger-print: finger-print is differentiated the peak relative retention time: schizandrin 1.00, wuweizi alcohol B 1.25, Ge Mixin N/ isomeride 1.63, schizandrin A 1.88, Ge Mixin N/ isomeride 3.18, deoxyschizandrin 3.27; (5) fruit of Chinese magnoliavine plantation collecting method; The present invention can control the quality of raw material comprehensively, guarantees the steady quality of product.

Description

Schisandra raw material fingerprint quality determining method in the body resistance-strengthening stasis-eliminating plant drug
Technical field
The invention belongs to schisandra raw material quality determining method field, particularly relate to schisandra raw material fingerprint quality determining method in a kind of body resistance-strengthening stasis-eliminating plant drug.
Background technology
The fruit of Chinese magnoliavine (Fructus Schisandrae chinensis) is the dry mature fruit of Magnoliaceae (Magnoliaceae) the schisandra plant fruit of Chinese magnoliavine [Schisandra chinensis (Turcz.) Baill.].The fruit of Chinese magnoliavine has another name called dark plum, mountain flower green pepper, bower actinidia fruit, gains the name because of it has sweet, sour, hot, bitter, the salty five tastes, is stated from Shennong's Herbal the earliest, and be listed in top grade, also on the books in " figure is through book on Chinese herbal medicine ".
" Chinese Plants will " is described the fruit of Chinese magnoliavine and is the fallen leaves woody climbers, except that the spire back side by surplus nothing pubescence and perula tool echinid mao.Flower mostly is unisexuality, the Hua Dansheng or the axil of growing thickly, male flower: the long 5-25 millimeter of bennet, perianth white powder or pink, 6～9; Stamen is about 2 millimeters, and flower pesticide is about 1.5 millimeters, the extremely short filigree of no filigree or outer 3 pieces of stamen tools, connective is recessed or protrude blunt tip slightly, and 5 (6) pieces on stamen is mutually by pasting, uprightly be arranged in the top of the column holder that is about 0.5 millimeter, form the nearly oecium of falling the oval; Female flower: the long 17-38 millimeter of bennet, tapel is similar with male flower, the gynoecium ellipse, long 2-4 millimeter is from giving birth to carpel 17～40.The long 1.5-8.5 of aggregate fruit centimetre, the long 1.5-6.5 of polymerization carpopodium centimetre; Little berry is subsphaeroidal or fall oval, redness when ripe.Seed 1～2, kidney shape is filbert glossy.5～July of florescence, really 7～October of phase.
In the other shrub of cheuch, hillside, border and the small stream of fruit of Chinese magnoliavine self-sow below height above sea level 1700m.Be distributed in ground such as northeast, North China, the Inner Mongol, Ningxia and Henan.In the temperate zone, all there is distribution in warm temperate zone or mountain region, subtropics.Like shady and cool moist climate, happiness illumination, cold-resistant, not water-fast soaking needs appropriateness hidden, and the seedling phase is avoided the burning sun irradiation especially.Loose to select, fertile, as to be rich in soil ulmin subacidity or the cultivation of neutral loam are advisable.The weather conditions of suitable growth are generally: 0～14 ℃ of average annual temperature, and 500～1000 millimeters of annual rainfalls, the coldest month samming-3 ℃～-22 ℃, samming was 20 ℃～28 ℃ in the hottest month.
The fruit of Chinese magnoliavine current wild and artificial cultivation are also deposited, main product in northeast, provinces and regions such as Hebei, Shanxi, Shaanxi, Ningxia, Shandong and the Inner Mongol.
The fruit of Chinese magnoliavine is mainly with fruit medicine, and " Chinese pharmacopoeia record schisandra chinensis medicinal material is irregular sphere or oblate spheroid, diameter 5～8mm.Surface redness, aubergine or kermesinus, shrinkage shows glossy, the pulp softness, the surface that has is dark red or appearance " bloom ".Seed 1～2, kidney shape, surperficial pale brown look, glossy, the kind skin is thin and crisp.Pulp gas is little, flavor acid; After the seed fragmentation, fragrance is arranged, flavor is hot, little hardship.
The fruit of Chinese magnoliavine is used as medicine with fruit and seed, and effective constituent is Lignanoids compounds, also contains chemical constitutions such as terpene, organic acid.The principal ingredient division is as follows:
A. Lignanoids compounds
At present, from schisandra plant, isolated 40 surplus kind of lignan compound monomer, wherein contain 32 kinds in the fruit of Chinese magnoliavine.At this surplus 40 in kind of the compound, have 10 kinds of clear and definite pharmacological action have been found, wherein 7 kinds are arranged in the fruit of Chinese magnoliavine, be respectively schizandrin A (Schizandrin A), deoxyschizandrin (Schizandrin B), schisandrin C (Schizandrin C), schizandrin (Schizandrol A), wuweizi alcohol B (Schizandrol B), Schisantherin C (Schisantherin A) and wuweizi ester B (Schisantherin B), all belong to the cyclohexyl biphenyl octene class in lignanoid's composition.And schisanhenol, Biao-Jia Baxin, anwulignan, 6-O-benzoyl Gomisin O, Ge Mixin N, root of Dahurain angelica acyl group gomisin H.
What Study on Physiological Activity was more in the lignanoids is to the effective composition of liver.To 7 kinds of effective constituent pharmacological researches of the fruit of Chinese magnoliavine and clinical proof, the effect that reduces the hepatitis serum GPT levels is all arranged, wherein the strongest with the wuweizi ester B effect, be pure second, third element, second element, first element, ester first and pure first secondly.It mainly is to hepatocellular protective effect that enzyme mechanism falls in the fruit of Chinese magnoliavine; can promote the hepatocellular reparation of damage or suppress liver cell lesion that make cell membrane that certain function take place and sexually revise, permeability reduces; thereby the transaminase that drains in the blood plasma is reduced, to the synthetic inhibiting effect that there is no of transaminase.In addition, find that also fruit of Chinese magnoliavine lignanoid composition has antioxidation, the strongest with the antioxidation activity of deoxyschizandrin.
B. terpenoid
Terpenoid mainly is present in the volatile oil of the fruit of Chinese magnoliavine, and fruit of Chinese magnoliavine cauline leaf, fruit and seed all contain abundant volatile oil.People such as Qin Bo identify 32 components from the volatile oil of the fruit of Chinese magnoliavine, mainly be monoterpenes, contain oxygen monoterpenes, sesquiterpenoids and contain the oxygen sesquiterpenoids, and are wherein maximum with the sesquiterpenoids material.Ke Ming reports Fructus Schisandrae Chinensis volatile oil tool antibechic effect clearly, and its effectiveness is 75% of codeine
C. other compositions
Schisandra fruit contains multiple organic acids such as citric acid, malic acid, succinic acid, tartrate, and tangible phlegm-dispelling functions is arranged.In addition, mineral matters such as sterol, vitamin C, E, resin, tannin and iron, manganese, silicon, phosphorus in schisandra fruit, have also been found.Also contain 7 kinds of monose, 17 seed amino acids and 16 kinds of trace elements such as glucose in the fructus schisandrae dry mature fruit, have anti-aging effects.
The effective constituent Lignanoids compounds of the fruit of Chinese magnoliavine is mainly derived from fruit and the seed of the fruit of Chinese magnoliavine, and traditional extracting method has alcohol extracting, chloroform extraction and water to extract the equal solvent extraction method.Fado rope solvent system extracted in recent years, supercritical CO 2Extractive technique and microwave auxiliary extracting method.Liu Ben etc. [2]Carried out research with schizandrin A in the fado rope solvent extraction fruit of Chinese magnoliavine, and the supercritical CO of regulating with 10% methyl alcohol 2Extraction ratio compare.Supercritical CO with the adjusting of 10% methyl alcohol 2Extraction ratio compare, fado rope solvent can obtain about 94% extraction recovery.Zhou Qinghua [3], Yang Subei [4], Xiang Zhimin etc. [5]All investigated supercritical CO 2Extracting method is to extraction efficiency, and extraction conditions is optimized.Huang Huihua etc. [6]Study the microwave auxiliary extracting method of schizandrin in the schisandra fruit, investigated various extraction conditions, obtained best microwave-assisted extraction process.Other extracting method such as percolation, ultrasonic method also have relevant report.
The method for separating and detecting of schisandra lignan chemical constitution mainly contains spectrophotometric method [7] ~ [11], high performance liquid chromatography [12] ~ [22], thin-layered chromatography [23] ~ [24], wherein using maximum analytical approachs is high performance liquid chromatography.Document is arranged in addition [25]Reported application GC-MS method and CEC method separation detection to the schisandra lignan chemical constitution.Stipulated the assay method of the HPLC of schizandrin at Chinese Pharmacopoeia (2005).
About the research of fruit of Chinese magnoliavine finger-print, people such as Chen Hongxuan [26], Shi Jiaping [27], people such as Feng Xuesong [28], people such as Yin Fangzhou [29]All the finger-print of schisandrol soluble components is studied, and with the lignan component schizandrin, schizandrin A, deoxyschizandrin are reference substance.And people such as Li Yanli [30], people such as Feng Wei [31]Finger-print to fruit of Chinese magnoliavine water soluble ingredient is studied.People such as Fan Zhuowen [32]Then investigated the finger-print of schisandra chinensis medicinal material Different Extraction Method, schisandra chinensis medicinal material is respectively through chloroform, methyl alcohol, and ethanol, 50% ethanol, water extracts and CO 2Supercritical extract.
Present quality control about the fruit of Chinese magnoliavine mainly is single or certain several composition is main, can not react the global feature of medicinal material, finger-print provides such method, the index that the single index components or the active component of routine is quality control rises to a new stage, fingerprint characteristic with chromatogram, with the quantization parameter that obtains by finger-print, more effectively discern the false from the genuine control of quality.
Finger-print about schisandra chinensis medicinal material also has some research reports, but is not very perfect, the quality control that is not applied to produce Chinese crude drug.Simultaneously according to existing chemical constitution of the fruit of Chinese magnoliavine and pharmacology clinical research data, and the supporting vital QI and dispersing blood stasis pharmacological research is with the achievement in research of effective constituent, determine that the active site and the main active that need to characterize are lignanoids, so requirement can embody the global feature of lignan component in the schisandra chinensis medicinal material all sidedly.Adopt the LC-MS technology that the main chromatographic peak in the finger-print is belonged to, guaranteed that effective constituent is demonstrated fully in the fruit of Chinese magnoliavine in finger-print.
Summary of the invention
Technical matters to be solved by this invention provides schisandra raw material fingerprint quality determining method in a kind of body resistance-strengthening stasis-eliminating plant drug preparation, and this method can be controlled the quality of raw medicinal material comprehensively, guarantees the steady quality of product.
Technical scheme of the present invention is as follows:
The schisandra raw material fingerprint quality determining method comprises the following steps: in a kind of body resistance-strengthening stasis-eliminating plant drug
(1) extracts fruit of Chinese magnoliavine test sample
Take by weighing 0.5g schisandra chinensis medicinal material powder, add 20ml 80% methyl alcohol, claim to decide weight, ultrasonic Extraction 20-50min supplies institute's weight loss, through 0.23-0.45 μ m filtering with microporous membrane, gets need testing solution;
(2) gradient elution moving phase
With octadecylsilane chemically bonded silica is filling agent, and water and acetonitrile are that moving phase is carried out wash-out moving phase, and chromatographic column is Eclipse; Mobile phase A is water mutually, and B is acetonitrile mutually; Gradient elution: 0-40min, 40-80%B; Flow velocity 0.8-1.2ml/min; Detect wavelength 210-280nm; Column temperature 20-40 ℃; Sample size 10-20ul.
Condition of gradient elution is:
Time (min) A phase: water (%) B phase: acetonitrile (%)
0 60 40
40 20 80
(3) foundation of standard finger-print
Choose the sample of 10 batches of different lot numbers, carry out the efficient liquid-phase chromatograph finger print atlas analysis.All peaks in the HPLC finger-print of appropriate samples are compared, determined 10 total peaks, and be numbered (Fig. 1) by appearance time precedence.
In total peak, choose 7 characteristic peaks, be respectively No. 1 peak schizandrin, No. 3 peak wuweizi alcohol Bs, No. 4 peak Ge Mixin N/ isomeride, No. 6 peak schizandrin As, No. 7 peaks and No. 8 peak Ge Mixin N/ isomeride, No. 9 peak deoxyschizandrins.Wherein deoxyschizandrin is an important activity composition.
According to the qualification result of LC-MS-MS, the efficient liquid-phase chromatograph finger print atlas of the fruit of Chinese magnoliavine has been expressed the distribution character of lignanoid.Choose the higher schizandrin of content as the index components peak.
Process is to the research of the schisandra chinensis medicinal material finger-print of Liaoning, Heilungkiang, a plurality of places of production, Jilin ten batch samples, the finger-print of choosing a collection of schisandra chinensis medicinal material according to following principle is finger-print (Fig. 1) in contrast: in conjunction with the effect experiment situation, pay the utmost attention to the finger-print of the medicinal material of determining curative effect.Finger-print and quantitative measurement result are compared, reject irrational especially sample, pay the utmost attention near the finger-print of the sample of content mean value.In conjunction with finger-print and quantitative result, the selected characteristic peak separates better, and the retention time at peak and peak height are suitable, the typical finger-print of peak type (shape at peak and peak height ratio).Preferentially choose the finger-print that baseline is steady, signal to noise ratio (S/N ratio) is good;
(4) quality control of finger-print
A. the discriminating of the sample true and false
Calculate the relative retention time RRT (retention time at the retention time of RRT=characteristic peak/index peak) of each characteristic peak in ten batches of medicinal materials fingerprints according to formula, in conjunction with two breadboard checking results, determined the relative retention time and the scope (table 1) of each characteristic peak.
6 finger-prints are differentiated the peak relative retention time: schizandrin 1.00, wuweizi alcohol B 1.25, schizandrin N/ isomeride 1.63, schizandrin A 1.88, schizandrin N/ isomeride 3.18, deoxyschizandrin 3.27.
Table 1 schisandra chinensis medicinal material HPLC finger-print is differentiated peak relative retention time and scope
Figure C20071004033100071
Figure C20071004033100081
According to experiment condition testing sample is measured, drawn the HPLC chromatogram of sample, calculate the relative retention time of each characteristic peak, and compare with listed reference fingerprint and relative retention time table.All exist as each characteristic peak, and relative retention time (RRT) is identical, then can be defined as this raw material.
B. sample quality evaluation
Adopt traditional Chinese medicine fingerprint area of computer aided similarity evaluation software (Chinese Pharmacopoeia Commission), the HPLC finger-print and the reference fingerprint (or reference substance common pattern finger-print) of sample compared.Should be with the similarity that 10 total peaks calculate less than 0.9.
The relative retention time of table 2 characteristic peak and relative peak area
Figure C20071004033100082
* the retention time at the retention time of RRT (relative retention time)=characteristic peak/index peak
* the peak area at the peak area of RPA (relative peak area)=characteristic peak/index peak
Figure C20071004033100083
Described step 2 chromatographic column is Eclipse (150 * 4.6mm, 5 μ m); Flow velocity 1.0ml/min; Detect wavelength 254nm; 35 ℃ of column temperatures; Sample size 20ul.
Described step 4 by at least three batch samples are measured, is calculated correlation parameter after the determining fingerprint pattern condition is determined, and proposes the suitable parameters condition of highly effective liquid phase chromatographic system on this basis.The chromatographic peak area reappearance (RSD) that is schizandrin reference substance solution (100 μ g/ml) is not higher than 3%, and retention time reappearance (RSD) is not higher than 2%; The degree of separation of schizandrin and adjacent peak is not less than 1.0; The chromatographic column post is imitated and is no less than 30,000 theoretical cam curves in schizandrin.
Another technical scheme of the present invention is as follows
The plantation collecting method of schisandra raw material comprises the following steps: in a kind of body resistance-strengthening stasis-eliminating plant drug
(1) GAP of schisandra chinensis medicinal material
Northeast fruit of Chinese magnoliavine spring in next year (early April) is taken out vernalization in the chamber that is placed on about room temperature 15-20 ℃, seed breach after several days, and plumule just exposes, and can sow.To be that layer below trips out seedling with sharp spade edge from an end in seedbed during lifting.Generally transplant in the first tenday period of a month in late April to May;
Be anti-spring drought the Spring Festival, general week sprinkling irrigation once (is decided on soil meterological condition).The principle of topdressing is based on the farm manure that becomes thoroughly decomposed, and is aided with chemical fertilizer.Fruit of Chinese magnoliavine branch spring, summer, Qiu Sanji all can prune.The fruit of Chinese magnoliavine is a liana, can not independently grow, and transplants and promptly answers built in back 1 year.
(2) standardization of schisandra chinensis medicinal material is gathered
The fruit of Chinese magnoliavine autumn results, (generally annual September first arrival the Frost's Descent before and after) fruit deliquescing and high resilience in the fall, outward appearance takes on a red color or during aubergine, timely collecting.Gather fine or cloudy, cut along the fruit ear root, put into clean basket with secateurs.Dry or dry in the shade.If harvest yield is big or the chance rainy day can dry by the fire with low baking temperature, the fruit ear of gathering back is placed on the fruit stack, removes branches and leaves, carpopodium and other impurity.The fruit stack is put on the shelf of baking, heated to about 50 ℃, baking is cooled to about 30 ℃ during to the half-dried left and right sides, when reaching eighty per cant when doing (about moisture 25%), the fruit of Chinese magnoliavine is moved to outdoor solarization to absolutely dry.
Beneficial effect of the present invention is as follows:
1, the finger-print of schisandra chinensis medicinal material can embody the global feature of lignan component in the schisandra chinensis medicinal material all sidedly.Adopt the LC-MS technology that the main chromatographic peak in the finger-print is belonged to, guaranteed that effective constituent is demonstrated fully in the fruit of Chinese magnoliavine in finger-print.
2, investigated the stability of need testing solution, the result shows, at room temperature, within 24 hours, it is stable that fruit of Chinese magnoliavine need testing solution keeps.The stability of sample in 1 year of the company of investigation simultaneously storage finds that similarity is greater than 0.9.Precision and replica test show that all similarity is more than 0.99.
3, the construction with finger-print and medicinal material GAP base combines, and just begins to control the quality of medicinal material in medicinal material production, has guaranteed the enforcement of finger-print like this, instructs the construction in GAP base, and really applies to quality of medicinal material control.
4,, find that the medicinal material similarity is greater than between the 0.9-1.0 through the finger-print similarity of the ten batches of schisandra chinensis medicinal materials in schisandra chinensis medicinal material base, northeast is calculated.The fruit of Chinese magnoliavine finger-print quality control method of setting up is described, highly sensitive, good reproducibility, specificity is strong, and is easy and simple to handle, and method is reliable, can fruit of Chinese magnoliavine quality carry out science, effectively evaluating confirms to apply to quality control in the actual production, satisfies the demand of medicinal material discriminating and quality control.
5. quality of medicinal material is stable, simultaneously the stable and controllable of the supporting vital QI and dispersing blood stasis quality of the pharmaceutical preparations that also guarantees.
Description of drawings
The typical fruit of Chinese magnoliavine efficient liquid-phase chromatograph finger print atlas of Fig. 1
The finger-print of Fig. 2 fruit of Chinese magnoliavine sample
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Schisandra chinensis medicinal material: Northeast China (10 batches)
Instrument
Figure C20071004033100101
Take by weighing 0.5g schisandra chinensis medicinal material powder, add 20ml 80% methyl alcohol, claim to decide weight, ultrasonic Extraction 50min supplies institute's weight loss, through 0.45 μ m filtering with microporous membrane, gets need testing solution.Chromatographic condition: column temperature: 35 ℃, detect wavelength: 254nm, sample size: 20 μ l, chromatographic column: Eclipse (150 * 4.6mm, 5 μ m), elution requirement (seeing Table 1)
Table 1 elution requirement
Time (min) A phase: water (%) B phase: acetonitrile (%) Flow velocity (ml/min)
0 60 40 1.0
40 20 80 1.0
After the determining fingerprint pattern condition is determined, by at least three batch samples are measured, calculate correlation parameter, and propose the suitable parameters condition of highly effective liquid phase chromatographic system on this basis.The chromatographic peak area reappearance (RSD) that is schizandrin reference substance solution (100 μ g/ml) is not higher than 3%, and retention time reappearance (RSD) is not higher than 2%; The degree of separation of schizandrin and adjacent peak is not less than 1.0; The chromatographic column post is imitated and is no less than 15,000 theoretical cam curves in schizandrin.
By the similarity of ten batches of schisandra chinensis medicinal materials is calculated, find that the medicinal material similarity is greater than between the 0.9-1.0.The fruit of Chinese magnoliavine finger-print quality control method of setting up is described, easy and simple to handle, method is reliable, and confirmation can apply to quality control in the actual production, satisfies the demand of medicinal material discriminating and quality control.
A collection of schisandra chinensis medicinal material sample fingerprint image spectrogram is seen Fig. 2, and the relative retention time and the relative peak area of characteristic peak see Table 2.

Claims (3)

1. schisandra raw material fingerprint quality determining method in the body resistance-strengthening stasis-eliminating plant drug comprises the following steps:
(1) extracts the fruit of Chinese magnoliavine
Take by weighing 0.5g schisandra chinensis medicinal material powder, add 20ml 80% methyl alcohol, claim to decide weight, ultrasonic Extraction 20-50min supplies institute's weight loss, through 0.23-0.45 μ m filtering with microporous membrane, gets need testing solution;
(2) gradient elution moving phase
With octadecylsilane chemically bonded silica is filling agent, and water and acetonitrile are that moving phase is carried out gradient elution, and chromatographic column is Eclipse; Mobile phase A is water mutually, and B is acetonitrile mutually; Gradient elution: 0-40min, 60-20%A, 40-80%B; Flow velocity 0.8-1.2ml/min; Detect wavelength 210-280nm; Column temperature 20-40 ℃; Sample size 10-20ul;
(3) foundation of standard finger-print
10 total peaks have been determined, 7 characteristic peaks have been chosen, be No. 1 peak schizandrin, No. 3 peak wuweizi alcohol Bs, No. 4 peak Ge Mixin N/ isomeride, No. 6 peak schizandrin As, No. 7 peaks and No. 8 peak Ge Mixin N/ isomeride, No. 9 peak deoxyschizandrins, wherein deoxyschizandrin is an important activity composition;
Choose the higher schizandrin of content as the index components peak;
Pay the utmost attention to the finger-print of the medicinal material of determining curative effect; Pay the utmost attention near the finger-print of the sample of content mean value; In conjunction with finger-print and quantitative result, the selected characteristic peak separates better, and the retention time at peak and peak height are suitable, the typical finger-print of peak type; Preferentially choose the finger-print that baseline is steady, signal to noise ratio (S/N ratio) is good;
(4) quality testing of finger-print
A. the discriminating of the sample true and false
6 finger-prints are differentiated the peak relative retention time: schizandrin 1.00, wuweizi alcohol B 1.25, Ge Mixin N/ isomeride 1.63, schizandrin A 1.88, Ge Mixin N/ isomeride 3.18, deoxyschizandrin 3.27;
B. sample quality evaluation
The HPLC finger-print and the reference fingerprint of sample are compared, should be with the similarity that 10 total peaks calculate less than 0.9.
2. schisandra raw material fingerprint quality determining method in the body resistance-strengthening stasis-eliminating plant drug according to claim 1 is characterized in that: described step 2 chromatographic column is Eclipse150 * 4.6mm, 5 μ m; Flow velocity 1.0ml/min; Detect wavelength 254nm; 35 ℃ of column temperatures; Sample size 10-20ul.
3. schisandra raw material fingerprint quality determining method in the body resistance-strengthening stasis-eliminating plant drug according to claim 1, it is characterized in that: the quality testing of the finger-print in the described step (4) is under the determining fingerprint pattern condition, by at least three batch samples are measured, the chromatographic peak area reappearance RSD of schizandrin reference substance solution 100 μ g/ml is not higher than 3%, and retention time reappearance RSD is not higher than 2%; The degree of separation of schizandrin and adjacent peak is not less than 1.0; The chromatographic column post is imitated and is no less than 30,000 theoretical cam curves in schizandrin.
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