CN105606752A - Detection method of fingerprint spectrums of sugar-free strong pipa syrup - Google Patents
Detection method of fingerprint spectrums of sugar-free strong pipa syrup Download PDFInfo
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- CN105606752A CN105606752A CN201610045155.6A CN201610045155A CN105606752A CN 105606752 A CN105606752 A CN 105606752A CN 201610045155 A CN201610045155 A CN 201610045155A CN 105606752 A CN105606752 A CN 105606752A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention provides a detection method of fingerprint spectrums of sugar-free strong pipa syrup. The fingerprint spectrums of various ingredients in the sugar-free strong pipa syrup are detected and obtained. The sugar-free strong pipa syrup standard spectrums obtained through the method can provide a reliable basis for identifying the sugar-free strong pipa syrup and controlling quality.
Description
Technical field
The invention provides a kind of Sugarless type intensified loquet distillate fingerprint atlas detection method, belong to medical technical field.
Background technology
Intensified loquet distillate is for conventional Chinese patent drug, by loguat leaf, the tuber of stemona, Cynanchum glaucescens, menthol, pappy shell, the root bark of white mulberry, balloonflower root 7Taste Chinese medicine composition, has that yin-nourishing is astringed the lung, antibechic, the effect of eliminating the phlegm, for chronic cough due to asthenia of viscera, bronchitis etc.
1, loguat leaf is conventional Chinese medicine simply, its bitter, micro-pungent, cold nature. Attach to the lung and stomach meridians, be just taken as since ancient timesMedicinal material uses, and is traditional relieving cough and asthma Chinese medicine, has preventing phlegm from forming and stopping coughing, harmonizing stomach and lowering adverse Qi, effect of dysentery diuresis only, to neuralgia, passJoint inflammation, Low Back Pain and cancer etc. also have certain curative effect. Also cure mainly the diseases such as cough with lung heat, deficiency of Yin phthisical cough, eczema, record in go through version " inState's pharmacopeia " for tcm clinical practice.
The chemical composition of loguat leaf comprises: (1) triterpenes: the triterpene compound in loguat leaf have betulinic acid methyl esters,Oleanolic acid, malol (ursolic acid), 2-α hydroxyl oleanolic acid methyl esters, Corosolic acid methyl esters, 2-α hydroxyl oleanolic acid, section sieveRope acid, tormentic acid, euscaphic acid etc.; At present, more to triterpene acids loquat leaf research is mainly ursolic acid and oleanolic acid. (2)Flavonoids: contain multiple chromocor compound in loguat leaf, its aglycon is mainly kaempferol, Quercetin, glucosides is by 1-3 monose groupBecome, common aglycon is glucose, rhamnose, galactolipin, arabinose, and link position mostly is 3-position, also has a small amount of acetylationFlavonoid glycoside exists. (3) other compositions: the compositions such as sesquiterpenoids, Polyphenols.
2, Chinese medicine pappy shell is the ripe shell of bloodroot opium poppy, have astringe the lung, the function of puckery intestines, pain relieving, for for a long timeCough, rush down for a long time, prolapse of the anus, epigastric pain. The contained main bioactive ingredients of pappy shell is opiates, takes for a long time easy habituation.
Pappy shell chemical composition: (1) morphine hydrochloride: belonging to opiates alkaloid, is opioid receptor agonist. (2) phosphoric acidCodeine: chemistry 17-methyl-3-by name methoxyl group-4,5a-epoxy-7,8-bis-dehydrogenation morphinan-6a-alcohol phosphate sesquialter waterCompound. (3) papaverine hydrochloride: chemical name is: 1-[(3,4-Dimethoxyphenyl) methyl]-6,7-dimethoxy-isoquinoline saltHydrochlorate. (4) other compositions: also contain the alkaloids such as thebaine, narcotine and narcotoline in pappy shell.
3, the root bark of white mulberry is the dry root skin of moraceae plants mulberry. Root bark of white mulberry taste is sweet, pungent, cold in nature, has removing heat from lung and relieving asthma, Li Shui disappearsSwollen effect, is used for the treatment of dyspnea and cough due to lung-heat, oedema, turgor, oliguria, the diseases such as appearance skin edema.
Root bark of white mulberry chemical composition: (1) Coumarins: 5, umbelliferone, umbelliferone, Scopoletin, skimmi,Scopolactone (6-methoxyl group-7-hydroxyl-cumarin). (2) flavone compound: Cortex Mori element, ring morusin, mulberryElement, mulberrochromene, cyclomulberrin, cyclomulberrochromene element, morindone A-V, hydroxyl dihydro morusin, morusin-4-glucoside, mulberry skinRoot element hydroperoxides, compd A, Sang Genpi alcohol, ring mulberry tryptophol, mulberry glycosides A-D, the chalcone A that rubs, 5,7-dihydroxy chromone, twoHydrogen flavonoids sanggenon. (3) fragrant benzofuran derivative: be mainly mulberry skin furans A-Z, this compounds taking benzofuran asBasic structure. (4) polysaccharide: mucoitin, mulberry polysaccharide, chitin, shitosan. (5) other organic compounds: butanols, moracin(A, B, C, D, F, G), PCA ethyl ester, the acid of birch skin, glycoside derivative, cupreol, tannin and volatilization wet goods.
4, balloonflower root [Platycodongrandiflorum (Jacq.) A.DC.] is the dry root of Campanulaceae balloonflower root,Bitter, pungent, property is flat, returns lung channel, a surname's lung eliminates the phlegm, and is longer than a surname's lung and dispelling wind pathogens, for control catch cold or cough that wind-heat causes,The common medicines such as abscess of throat.
Balloonflower root chemical composition: (1) triterpenoid saponin: the main active ingredient of balloonflower root is platycodin, accounts for 2.5%. So farGot 18 kinds of triterpenoid saponins such as platycodin A, C, D, D2, D3, and Platycodin D is the main saponin(e in platycodin. (2)Flavonoids: Taxifolin, Quercetin-7-O-glucoside, Quercetin-7-O-rutinoside, wooden slippers grass-7-O-glucoside etc.(3) other compositions: phenols, carbene class, volatile oil, aliphatic acid, amino acid, mineral matter class etc.
5, the tuber of stemona is the piece root of Stemonaceae radix stemonae sessilifoliae, Radix stemonae japonicae and radix stemonae tuberosae, main product in Shandong, Anhui, riverThe ground such as Soviet Union, Hunan. Sweet, bitter, tepor, returns lung channel. There is effect of moistening lung to lower qi cough-relieving, desinsection. Cure mainly: cough due to wind-cold evil, one hundred daysCough, pulmonary tuberculosis, old age cough breathe heavily, roundworm disease, enterobiasis, skin mange, eczema etc.
Tuber of stemona chemical composition: the main component of the tuber of stemona is alkaloids, the up to the present tuber of stemona biology of definite structureAlkali has kind more than 100; (1) radix stemonae sessilifoliae root contains: tuberostemonine, stemonine, protostermonine, Stemonidine, the former stemonidine of dehydrogenationAlkali, different protostermonine, maistemonine, sessilistemonine A, sessilistemonine B, sessilistemonine C, sessilistemonine D, dihydroStemoninine, two deoxidation stemoninine A, two deoxidation stemoninine, stemoninine A, stemoninine B, stemoninine etc. (2) climingThe root of the raw tuber of stemona contains: stemonine, protostermonine, stenine alkali, sinostemonine, inferior stemonine, different stemonine, stemonamineAnd isotuberostemonine etc. (3) root of radix stemonae tuberosae contains: stemonine, tuberostemonine, isotuberostemonine, this is for peaceful alkali, inferiorTuberostemonine, oxidation radix stemonae tuberosae, stemine and this are for peaceful alkali etc.
6, peppermint is China's traditional Chinese medicine, is distributed widely in the Temperate Region in China in the Northern Hemisphere, is widely distributed in north and south each province in China.The peppermint genus wide in variety East Asia of China's cultivation and the peppermint kind of Tropical Asia. Peppermint medicinal material is that the ground of labiate peppermint is dryDry part, taste is pungent, cool in nature, oral for anemopyretic cold, wind-warm syndrome from the beginning of, headache, hot eyes, larynx numbness, order sore, rubella, measles, the chest side of bodySwollen vexed.
Peppermint chemical composition: the composition of peppermint is mainly Herba Menthae Haplocalycis volatile oil and menthol (menthol).
7, Cynanchum glaucescens is dry rhizome and the root of Asclepiadaceae plant rhizoma et radix cynanchi stauntoni or leaves of Daphne genkwa Cynanchum glaucescens, has sending down abnormally ascending, dissolving phlegm, stopsThe function of coughing, is mainly used in lung qi and stops up in fact, cough ant phlegm, and fullness sensation in chest is breathed heavily the anxious disease of waiting.
Cynanchum glaucescens chemical composition: (1) rhizoma et radix cynanchi stauntoni: Qiu Shengxiang is separated to 3 compositions, warp from the liposoluble constituent of its rhizomeSpectrum analysis is accredited as cupreol, C24～C30Aliphatic acid and triterpene hancockinol. (2) North China Cynanchum glaucescens: Lou Hongxiang etc. are from ChinaIn the Cynanchum glaucescens of north, separate to obtain two kinds of luxuriant and rich with fragrance indoles connection pyridine Alkaloids, by definite structures such as high resolution NMR spectrum, CD, ORD beAntofine and 6-go first peace holder point, after be further separated to again 5 compounds, be respectively sucrose, cupreol, daucosterol,The derivative C of sinapic acid and modification pregnane21Steroidal glycoside---radix cynanchi atrati glycosides first. Within 1991, they are therefrom separated to 4 new threeTerpenoid, by spectrum analysis and the relevant philosophy of chemistry be accredited as hancockinol, Hancolupenol, hancolupenone andHancolupenol octacosanate, is Novel framework compound, after separate again to obtain the monoterpene glycoside compound of a new construction,Name 3-oxygen-(β-D-xylopyranose(1～6)β-D-glucopyranosyl)-linalool. Within 1992, they are from the dry root of North China Cynanchum glaucescensEthanol extract in separate obtain 5 monoterpenes compounds, wherein 3 noval chemical compounds are 4-p-camphane-1,7,8 ,-triol,North China Cynanchum glaucescens Neogroside A and North China Cynanchum glaucescens new glycoside B, known compound is 4-p-lauro lene-1-8,9-glycol and 4-p-camphane-1,8,9Triol, after from the ethanol extract of its dry root, separate and identified 6 C again21Steroid compound, wherein glaucogenin C is whiteCommon vetch glycosides A, Cynanchum glaucescens aglycon A, dehydration He La get aglycon is known compound; Noval chemical compound is North China Cynanchum glaucescens aglycon B, North China glaucosideA。
At present little about the fingerprint identification document of intensified loquet distillate, Chinese patent application CN201010263871.4The content assaying method of morphine in a kind of thin-layer chromatography authentication method of loguat leaf and pappy shell is disclosed. Chinese patent applicationCN201210312564.X, discloses the authentication method of three kinds of compositions of intensified loquet distillate, comprises pappy shell, menthol, loquatThe thin-layered chromatography qualification of leaf, the liquid chromatography for measuring of pappy shell content. Chinese patent application CN200610018599, openA kind of thin-layer chromatography authentication method of menthol.
Said method all can not be measured all the components of intensified loquet distillate simultaneously, but can only measure certain composition, andThere is inexactness in thin-layered chromatography.
Finger-print is taking multicomponent as index, the effective ways of overall merit Chinese medicine and Chinese patent drug inherent quality, in201410682971.9 1 kinds of intensified loquet distillate fingerprint pattern quality control methods of state's patent, the method adopts high performance liquid chromatographyMethod, first criticizes brute force and is optimized revealing preparation method and the chromatographic condition of product solution to be measured, comprise mobile phase system,Eluent gradient, extract solvent, extraction time etc., make that chromatogram separates better, spectrum peak information content more, that provide is larger;Then optimize detection wavelength, obtained baseline intensified loquet distillate sample chromatogram figure stably.
Intensified loquet distillate is by loguat leaf, pappy shell, the tuber of stemona, the root bark of white mulberry, balloonflower root, Cynanchum glaucescens and menthol seven flavor medicine material groupBecome, have that yin-nourishing is astringed the lung, the merit of kobadrin, chatter and cough for chronic cough, bronchitis etc. Because one-tenth is grouped into complexity, effectively becomeThe diversity of dividing, requires further to improve to the post effect of chromatogram, not only needs separating degree high, highly sensitive, and processing speedAlso need further to improve. Therefore, for reflecting more exactly the total quality situation of intensified loquet distillate, except to wherein many groupsPoint, outside many indexs control, be necessary that research sets up the finger-print of more reliable intensified loquet distillate.
Summary of the invention
The object of the invention is to overcome the defect of prior art, set up more accurate, the reliable and efficient Sugarless type of oneIntensified loquet distillate finger print atlas identifying method, the method can be used for differentiating the quality of Sugarless type intensified loquet distillate, the invention providesSet up a method for Sugarless type intensified loquet distillate finger-print, the preparation of test sample comprises the following steps:
1) intensified loquet distillate intermediate: except menthol, the Six-element medicinal material boilings twice such as all the other loguat leaves, each2h, collecting decoction, filters, and filtrate is concentrated into about 750ml, obtains intensified loquet distillate intermediate;
2) preparation of intensified loquet distillate test sample: except menthol, the Six-element medicinal material boilings twice such as all the other loguat leaves,Each 2h, collecting decoction, filters, and filtrate is concentrated into about 750ml, adds Sodium Benzoate 2.5g, is stirred to dissolve, and adds Steviosin 2g,Continue to be heated to boil, keep 20 minutes, leave standstill, filter, add citric acid 0.5g, the appropriate and menthol of the essence that dissolves with ethanol,Stir, evenly, leave standstill, filter, add water to 1000ml, mix, obtain intensified loquet distillate sample;
3) test sample of loguat leaf, the tuber of stemona, Cynanchum glaucescens, the root bark of white mulberry and balloonflower root medicinal material is prepared as respectively by loguat leaf, the tuber of stemona, whiteBefore, the root bark of white mulberry and balloonflower root medicinal material boiling twice, each 2h, collecting decoction, filters, filtrate is concentrated, make respectively loguat leaf,The simple decocting liquid of the tuber of stemona, Cynanchum glaucescens, the root bark of white mulberry and balloonflower root.
Preferably,
The preparation of test sample is further comprising the steps of:
The preparation of object of reference solution: it is appropriate that precision takes Sodium Benzoate reference substance, adds methyl alcohol and is mixed with every 1ml and contains benzene firstThe object of reference solution of acid sodium 0.2mg;
The preparation of need testing solution: get respectively intensified loquet distillate sample, intensified loquet distillate intermediate, loguat leaf, the tuber of stemona, whiteBefore, the simple decocting liquid of the root bark of white mulberry and balloonflower root carries out respectively centrifugally, precision measures 1ml, upper in SPE solid phase extraction column(WelchromC18E500mg/6ml), water elution is settled in 5ml volumetric flask, shakes up, and 0.22 μ m miillpore filter filters, and gets continuousFiltrate, respectively intensified loquet distillate sample, intensified loquet distillate intermediate, loguat leaf, the tuber of stemona, Cynanchum glaucescens, the root bark of white mulberry and balloonflower rootSimple reference substance.
Preferably,
Accurate object of reference solution and the need testing solution 1 μ l of drawing, injects Ultra Performance Liquid Chromatography instrument, application respectivelyACQUITYUPLCBEHC18(2.1 × 100mm, m) chromatographic column of 1.7 μ; Record chromatogram, obtain corresponding need testing solutionChromatogram, sets up finger-print according to UPLC chromatography.
Preferably,
Mobile phase application methyl alcohol-0.1% formic acid system wash-out, column temperature is 35 DEG C; Flow velocity is 0.3ml/min;
Preferably, detecting wavelength is 254nm.
Preferably, by similarity evaluation, test sample finger-print and comparison film fingerprint imageSpectrum is calculated through similarity, and similarity must not be lower than 0.90.
Preferably, wherein the program of gradient elution is undertaken by following volume by volume concentration configuration: taking methyl alcohol as mobile phase A,0.1% formic acid is Mobile phase B,
Preferably, in described finger-print, there is the average retention time at the total peak of feature to comprise, 1.264,2.161,4.539、7.373、12.281。
Detailed Description Of The Invention
Detect the selection of wavelength
At present known and have composition morphine, codeine phosphate, papaverine hydrochloride, a former tuber of stemona of reference substance in intensified loquet distillateAlkali, tuberostemonine etc. Consider the maximum absorption wavelength that should as far as possible select these several compositions, respectively 210nm, 237nm,Collection of illustrative plates under 245nm, 254nm, 286nm, 300nm, the several wavelength of 330nm as a comparison, finally determines that wavelength 254nm is for detectingWavelength, the more and easy identification of chromatographic peak under this wavelength, baseline are also comparatively smooth. See that Fig. 1-1 is to Fig. 1-7.
The selection of flow phase system
Intensified loquet distillate contains seven flavor medicine material, complicated component, and polarity difference is larger, is necessary to apply gradient separations methodThe composition of most of various character is separated preferably, adopt ACQUITYUPLCBEHC18(2.1×100mm,1.7μM) chromatographic column, has carried out methyl alcohol-0.1% formic acid system, methyl alcohol-0.2% glacial acetic acid system, acetonitrile-0.1% formic acid system, firstThe investigation of alcohol-water system and methyl alcohol-0.2% trifluoroacetic acid system, result shows: application methyl alcohol-0.1% formic acid system wash-out canIntensified loquet distillate sample is separated preferably, and baseline is steady, peak shape is sharp-pointed, meets the requirement of finger-print. See Fig. 2-1To 2-5.
The setting of gradient condition
Intensified loquet distillate composition is more, and polarity difference adopts simple linear gradient as type of elution, not only compared with dieEasy to operate, 21 minutes time, A reaches 100% mutually, can effectively rinse chromatographic column, and chromatographic column can not produced because of continuous sample introductionSample is residual, affects the mensuration of next sample; With this understanding, can make most of chromatographic peak reach better separation, retention timeModerate, without wasting space, and 25 minutes after without other chromatographic peak. And can ensure the reappearance of finger-print, finally establishFixed condition makes the total composition of the overwhelming majority reach baseline separation, for further assay and other experiments provide good basePlinth. Refer to table 1
The selection of chromatographic column
Try out respectively ACQUITYUPLCBEHC18(2.1 × 100mm, 1.7 μ are chromatographic column, ACQUITYUPLC m)HSSC18(2.1 × 100mm, 1.8 μ are chromatographic column and TheromnSCIENTIFIC (m) chromatographic column of 100 × 2.1,1.7 μ, employing m)Above-mentioned definite flow phase system, the UPLC that carries out intensified loquet distillate sample analyzes. Under identical chromatographic condition, gained fingerprintSpectrum peak shape, retention time, separating degree have different, so need stationary chromatographic post. Result shows: ACQUITYUPLCBEHC18(2.1 × 100mm, 1.7 μ m) chromatographic column are better to the separating effect of the each composition of intensified loquet distillate, therefore determine that it is UPLC and refer toThe analysis chromatographic column of line collection of illustrative plates. See that Fig. 3-1 is to 3-3.
The selection of column temperature
In order to keep the uniformity of chromatography, column temperature is set is 35 DEG C and carry out chromatography, 35 DEG C are easy to control, and refer toLine collection of illustrative plates baseline is steady, and each component separation is effective. Once investigated 30 DEG C, 40 DEG C two column temperatures, after result column temperature changes, except protectingStay outside the time changes to some extent, chromatographic peak occurs overlapping, causes separating effect not good. Through considering, selecting column temperature is 35 DEG C, knotFruit sees that Fig. 4-1 is to 4-3.
The selection of flow velocity
Be provided with respectively 0.2ml/min, 0.3ml/min, tri-flow velocitys of 0.4ml/min. When flow velocity is 0.2ml/min, baseLine is steady not, and peak shape is not good; When flow velocity is 0.4ml/min, along with the shortening of retention time, some chromatographic peak is overlapping; StreamWhen speed is 0.3ml/min, finger-print baseline is steady, and each component separation effect is better, therefore selection flow velocity is 0.3ml/min, and knotFruit sees that Fig. 5-1 is to 5-3.
The selection of need testing solution preparation condition
Intensified loquet distillate active ingredient is comparatively complicated, in order effectively to be separated from intensified loquet distillate sample, and to otherClass material is removed as much as possible as Sodium Benzoate material, has adopted a herein, b, and c, tetra-kinds of methods of d are to intensified loquet distillate sampleCarry out pre-treatment, observe chromatographic peak and change, experimental technique is as follows:
A directly dilutes sample introduction
Precision measures the intensified loquet distillate sample 5ml making, and puts in 10ml volumetric flask and is diluted with water to scale, shake up,0.22 μ m miillpore filter filters, and gets subsequent filtrate, injects Ultra Performance Liquid Chromatography instrument, measures, and to obtain final product. See Fig. 6-1.
B extraction
1. precision measures intensified loquet distillate sample 25ml, adds strong ammonia solution 1ml, with ethyl acetate jolting extraction 6 times, each25ml, combined ethyl acetate liquid evaporate to dryness, residue adds methanol constant volume to 5ml measuring bottle, shakes up, and 0.22 μ m miillpore filter filters, and getsSubsequent filtrate, injects Ultra Performance Liquid Chromatography instrument, measures, and to obtain final product. See Fig. 6-2.
2. water liquid direct injected after extraction, water liquid is that step 1 extracts the lower layer of water liquid except ethyl acetate, 0.22 μ m microporeFilter membrane filters, and gets subsequent filtrate, injects Ultra Performance Liquid Chromatography instrument, measures, and to obtain final product. See Fig. 6-3.
The upper macroporous absorbent resin of c
Precision measures intensified loquet distillate sample 5ml, upper in D101 type large pore resin absorption column (internal diameter 2cm, 20cm), respectivelyWith 100ml water, 100ml50% ethanol and 100ml80% ethanol elution, collect respectively eluent, evaporate to dryness, residue adds water respectively,50% ethanol and 95% ethanol dissolve, and are settled in 5ml volumetric flask, shake up, and 0.22 μ m miillpore filter filters, and gets subsequent filtrate, noteExcess of imports high performance liquid chromatograph, measures, and to obtain final product. See Fig. 6-4,6-5,6-6.
The upper SPE solid phase extraction column of d
1. precision measures intensified loquet distillate sample 1ml, above (WelchromC on SPE solid phase extraction column18E500mg/6ml, 30PK), washing is put in 5ml measuring bottle and is mixed, and to obtain final product. See Fig. 6-7.
2. precision measures intensified loquet distillate sample 1ml, above (WatersSep-PakVac on SPE solid phase extraction columnC18-500mg), washing is put in 5ml measuring bottle and is mixed, and to obtain final product. See Fig. 6-8.
Result shows: intensified loquet distillate directly dilutes sample introduction and upper macroreticular resin preparation method and owes except Sodium Benzoate effectGood, SPE solid phase extraction column preparation method simple effectively except Sodium Benzoate effect still can, and can retain as much as possible effectivelyComposition, therefore select the method. This experiment adopts respectively WelchromC18-E500mg/6ml, 30PK and WatersSep-PakVacC18Two kinds of SPE solid phase extraction columns of-500mg, result is with WelchromC18E500mg/6ml, 30PK separating degree is better,Baseline is more steady.
The selection of object of reference
The preparation of object of reference in " technical requirement (provisional) of traditional Chinese medicine finger-print research ": formulating finger-print mustMust set up object of reference, should be according to the character of ingredient in test sample, select suitable reference substance as object of reference, in this experimentChoosing Sodium Benzoate (No. 7 peaks) is object of reference.
The preparation of object of reference solution
Precision adds methyl alcohol to be made every 1ml and contains 0.02mg Sodium Benzoate object of reference solution, the accurate object of reference solution, strong of drawingPower loquat dew need testing solution, carries out UPLC analysis, sees Fig. 7, Fig. 8.
Determine that in order to identify accurately and effectively the separation case of each chromatographic peak in finger-print 8 fingerprints have peak, logicalCross with reference substance and contrast, confirm that No. 7 peaks are Sodium Benzoate. See Fig. 9, the need testing solution of 10 batches of intensified loquet distillates, respectively according toThe preparation method of need testing solution obtains, and then analyzes according to UPLC condition, in table 11. Demarcate 8, total peak, each commonThere is peak relative retention time to be followed successively by: 1.264,2.161,4.539,5.266,7.373,7.609,12.281,17.075. And logicalCross and the retention time comparison of medicinal material, confirmed wherein 5 main peaks, wherein No. 1 peak is balloonflower root medicinal material, and No. 2 peaks are Cynanchum glaucescens medicineMaterial, No. 3 peaks are tuber of stemona medicinal material, and No. 5 peaks are root bark of white mulberry medicinal material, and No. 7 peaks are Sodium Benzoate.
Chromatographic condition: ACQUITYUPLCBEHC18(2.1 × 100mm, m) chromatographic column of 1.7 μ; Taking methyl alcohol as mobile phase A,0.1% formic acid is Mobile phase B, and the regulation according to the form below is carried out gradient elution, in table 11; Column temperature is 35 DEG C; Flow velocity is 0.2ml/Min; Refer to table 1.
The preparation of object of reference solution: it is appropriate that precision takes Sodium Benzoate reference substance, adds methyl alcohol and is mixed with every 1ml and contains benzene firstThe object of reference solution of acid sodium 0.2mg.
The preparation of need testing solution: get intensified loquet distillate sample centrifugal, precision measures 1ml, upper in SPE solid phase extraction column(WelchromC18E500mg/6ml), water elution is settled in 5ml volumetric flask, shakes up, and 0.22 μ m miillpore filter filters, and gets continuousFiltrate, to obtain final product.
Determination method: accurate object of reference solution and the each 1 μ l of need testing solution of drawing respectively, inject Ultra Performance Liquid Chromatography instrument,Record chromatogram, to obtain final product.
Press similarity evaluation, test sample finger-print to comparison film finger-print through similarDegree calculates, and similarity must not be lower than 0.90.
The method for building up of Sugarless type intensified loquet distillate finger-print of the present invention compared with prior art, has following excellentPoint:
By methodology checking and the survey to many batch samples of the investigation to finger-print testing conditions and acquisition processTry, finally set up the finger-print of intensified loquet distillate. By the investigation to finished product, medicinal material, intermediate correlation, finished product is referred toChromatographic peak in line collection of illustrative plates is followed the trail of and is confirmed. Like this, the quality standard by stable finger-print and after improving, makesThe quality of intensified loquet distillate is able to better control.
Brief description of the drawings
Fig. 1-1; The UPLC chromatogram that wavelength 210nm analyzes intensified loquet distillate
Fig. 1-2; The UPLC chromatogram that wavelength 237nm analyzes intensified loquet distillate
Fig. 1-3; The UPLC chromatogram that wavelength 245nm analyzes intensified loquet distillate
Fig. 1-4; The UPLC chromatogram that wavelength 254nm analyzes intensified loquet distillate
Fig. 1-5; The UPLC chromatogram that wavelength 286nm analyzes intensified loquet distillate
Fig. 1-6; The UPLC chromatogram that wavelength 300nm analyzes intensified loquet distillate
Fig. 1-7; The UPLC chromatogram that wavelength 330nm analyzes intensified loquet distillate
Fig. 2-1; Mobile phase is the UPLC chromatogram that methyl alcohol-0.1% formic acid is analyzed intensified loquet distillate
Fig. 2-2; Mobile phase is the UPLC chromatogram that methyl alcohol-0.2% glacial acetic acid is analyzed intensified loquet distillate
Fig. 2-3 mobile phase is the UPLC chromatogram that acetonitrile-0.1% formic acid is analyzed intensified loquet distillate
Fig. 2-4 mobile phase is the UPLC chromatogram that methanol-water is analyzed intensified loquet distillate
Fig. 2-5 mobile phase is the UPLC chromatogram that methyl alcohol-0.2% trifluoroacetic acid is analyzed intensified loquet distillate
Fig. 3-1ACQUITYUPLCBEHC18(2.1 × 100mm, 1.7 μ m) chromatographic column to intensified loquet distillate analyzeUPLC chromatogram
Fig. 3-2ACQUITYUPLCBEHPhenyl1.7 μ m2.1 × 100mm chromatographic column is to intensified loquet distillate analysisUPLC chromatogram
Fig. 3-3ACQUITYUPLCBEHPhenyl1.7 μ m2.1 × 100mm chromatographic column is to intensified loquet distillate analysisUPLC chromatogram
30 DEG C of UPLC chromatograms that intensified loquet distillate is analyzed of Fig. 4-1 column temperature
35 DEG C of UPLC chromatograms that intensified loquet distillate is analyzed of Fig. 4-2 column temperature
40 DEG C of UPLC chromatograms that intensified loquet distillate is analyzed of Fig. 4-3 column temperature
The UPLC chromatogram that Fig. 5-1 flow velocity 0.2ml/min analyzes intensified loquet distillate
The UPLC chromatogram that Fig. 5-2 flow velocity 0.3ml/min analyzes intensified loquet distillate
The UPLC chromatogram that Fig. 5-3 flow velocity 0.4ml/min analyzes intensified loquet distillate
Fig. 6-1 intensified loquet distillate directly dilutes the UPLC chromatogram that sample introduction is analyzed intensified loquet distillate
The UPLC chromatogram that Fig. 6-2 intensified loquet distillate ethyl acetate extraction sample introduction is analyzed intensified loquet distillate
The UPLC chromatogram that after the intensified loquet distillate ethyl acetate extraction of Fig. 6-3, water liquid sample introduction is analyzed intensified loquet distillate
The UPLC look that Fig. 6-semi-finals power loquat dew D101 type large pore resin absorption column water lotion sample introduction is analyzed intensified loquet distillateSpectrogram
Fig. 6-5 intensified loquet distillate D101 type large pore resin absorption column 50% ethanol sample introduction is analyzed intensified loquet distillateUPLC chromatogram
Fig. 6-6 intensified loquet distillate D101 type large pore resin absorption column 95% ethanol sample introduction is analyzed intensified loquet distillateUPLC chromatogram
The UPLC look that on the intensified loquet distillate of Fig. 6-7, SPE solid phase extraction column after washing liquid sample introduction is analyzed intensified loquet distillateSpectrogram
SPE solid phase extraction column after washing liquid sample introduction on Fig. 6-Final 8 power loquat dew
The UPLC chromatogram of Fig. 7 Sodium Benzoate
Fig. 8 intensified loquet distillate sample UPLC chromatogram
0 batch of intensified loquet distillate finger-print of Figure 91
Figure 10-1 loguat leaf medicinal material UPLC chromatogram
Figure 10-2 loguat leaf medicinal material and the contrast of intermediate UPLC chromatogram
Figure 10-3 loguat leaf medicinal material and intensified loquet distillate finished product UPLC chromatogram contrast contrast
Figure 11-1 tuber of stemona medicinal material UPLC chromatogram
Figure 11-2 tuber of stemona medicinal material and intermediate contrast
Figure 11-3 tuber of stemona medicinal material and finished product contrast
Figure 12-1 Cynanchum glaucescens medicinal material
Figure 12-2 Cynanchum glaucescens medicinal material and intermediate contrast
Figure 12-3 Cynanchum glaucescens medicinal material and finished product contrast
Figure 13-1 root bark of white mulberry medicinal material
Figure 13-2 root bark of white mulberry medicinal material and intermediate contrast
Figure 13-3 root bark of white mulberry medicinal material and finished product contrast
Figure 14-1 balloonflower root medicinal material
Figure 14-2 balloonflower root medicinal material and intermediate contrast
Figure 14-3 balloonflower root medicinal material and finished product contrast
Now the invention will be further described in conjunction with the accompanying drawings and embodiments:
Detailed description of the invention
Embodiment 1 sample determination
To 10 batches of intensified loquet distillate samples, measure brute force according to the UPLC finger-print condition of originally determiningThe main chromatographic peak relative retention time of loquat dew is as shown in table 2, and relative peak area is as shown in table 2, by UPLC chromatogram with *.ARW form is derived, and is led into TXT form, imports similarity evaluation system and compares analysis.
To number 1 sample as with reference to collection of illustrative plates, using above-mentioned 8 definite total peaks as check point, adopt " medianMethod " carry out the evaluation analysis of similarity. With reference to collection of illustrative plates and 10 batches of intensified loquet distillate sample finger-print match map, matching result is shown inTable 2-4.
Table 210 batch intensified loquet distillate determining fingerprint pattern result (relative retention time)
Table 310 batch intensified loquet distillate determining fingerprint pattern result (relative peak area)
Table 410 batch intensified loquet distillate similarity result of calculation
Can find out from above data result, the similarity of 10 batches of intensified loquet distillate samples is greater than 0.90, intensified loquet distillate sampleBetween product, there were significant differences, and chromatographic peak area RSD is 26.87%～45.26%.
Embodiment 2 intensified loquet distillate medicinal materials and finished product, intermediate correlation
The production technology of intensified loquet distillate except menthol, the Six-element medicinal material boilings twice such as all the other loguat leaves, each2h, collecting decoction, filters, and filtrate is concentrated into about 750ml, obtains the intermediate of intensified loquet distillate, and the intermediate of intensified loquet distillate addsSodium Benzoate 2.5g, is stirred to dissolve, and adds Steviosin 2g, continues to be heated to boil, and keeps 20 minutes, leaves standstill, and filters, and adds citric acid0.5g, the appropriate and menthol of the essence that dissolves with ethanol, stirs, and evenly, leaves standstill, and filters, and adds water to 1000ml, mixes, and to obtain final productFinished product intensified loquet distillate sample.
Intensified loquet distillate production technology and " preparation of solution " lower operation, self-control loguat leaf, hundred are pressed in the preparation of test sampleThe preparation of portion, Cynanchum glaucescens, the root bark of white mulberry and balloonflower root medicinal material is with reference to carrying out decocting preparation by intensified loquet distillate process for producing.
Decocting liquid, intermediate that the mensuration of finger-print is got intensified loquet distillate finished product, single medicinal material are all gone up in SPE solid phase and are extractedGet (WatersSep-PakVacC18-500mg) on pillar, washing is put in 5ml measuring bottle and is mixed, and to obtain final product.
Chromatographic condition: ACQUITYUPLCBEHC18(2.1 × 100mm, m) chromatographic column of 1.7 μ; Taking methyl alcohol as mobile phaseA, 0.1% formic acid is Mobile phase B, the regulation according to the form below is carried out gradient elution, sees the following form; Column temperature is 35 DEG C; Flow velocity is0.2ml/min; Gradient is as following table
UPLC gradient
The preparation of object of reference solution: it is appropriate that precision takes Sodium Benzoate reference substance, adds methyl alcohol and is mixed with every 1ml and contains benzene firstThe object of reference solution of acid sodium 0.2mg.
The preparation of need testing solution: get intensified loquet distillate sample centrifugal, precision measures 1ml, upper in SPE solid phase extraction column(WelchromC18E500mg/6ml), water elution is settled in 5ml volumetric flask, shakes up, and 0.22 μ m miillpore filter filters, and gets continuousFiltrate, to obtain final product.
Determination method: accurate object of reference solution and the each 1 μ l of need testing solution of drawing respectively, inject Ultra Performance Liquid Chromatography instrument,Record chromatogram, to obtain final product.
Press similarity evaluation, test sample finger-print to comparison film finger-print through similarDegree calculates, and similarity must not be lower than 0.90.
Sample introduction is measured respectively, detects by the intensified loquet distillate UPLC finger-print chromatographic condition of having set up, and obtains each medicinal materialUPLC finger-print, compares with intensified loquet distillate finger-print.
The correlation of loguat leaf medicinal material and finished product, intermediate
By the chromatogram of finished product, intermediate, loguat leaf medicinal material is made comparisons, No. 1 chromatographic peak in loguat leaf medicinal material existsIn finished product and intermediate, be also traceable to. These results suggest that loguat leaf medicinal material and intensified loquet distillate finished product, intermediate have wellCorrelation. See Figure 10-1,10-2,10-3.
The correlation of tuber of stemona medicinal material and finished product, intermediate
By the chromatogram of finished product, intermediate, tuber of stemona medicinal material is made comparisons, 1,2,3,4, No. 5 chromatogram in tuber of stemona medicinal materialPeak is also traceable in finished product and intermediate. These results suggest that tuber of stemona medicinal material and intensified loquet distillate finished product, intermediate have goodGood correlation. See Figure 11-1,11-2,11-3.
The correlation of Cynanchum glaucescens medicinal material and finished product, intermediate
By the chromatogram of finished product, intermediate, Cynanchum glaucescens medicinal material is made comparisons, 1 chromatographic peak in Cynanchum glaucescens medicinal material at finished product andIn intermediate, be also traceable to. These results suggest that Cynanchum glaucescens medicinal material and intensified loquet distillate finished product, intermediate have good correlation.See Figure 12-1,12-2,12-3.
The correlation of root bark of white mulberry medicinal material and finished product, intermediate
By the chromatogram of finished product, intermediate, root bark of white mulberry medicinal material is made comparisons, No. 1 chromatographic peak in root bark of white mulberry medicinal material existsIn finished product and intermediate, be also traceable to. These results suggest that root bark of white mulberry medicinal material and intensified loquet distillate finished product, intermediate have wellCorrelation. See Figure 13-1,13-2,13-3.
4.7.5 the correlation of balloonflower root medicinal material and finished product, intermediate
By the chromatogram of finished product, intermediate, balloonflower root medicinal material is made comparisons, No. 1 chromatographic peak in balloonflower root medicinal material is at finished productAnd be also traceable in intermediate. These results suggest that balloonflower root medicinal material and intensified loquet distillate finished product, intermediate have good relevantProperty. See Figure 14-1,14-2,14-3.
Embodiment 3 precision are investigated
Accurate absorption with a collection of intensified loquet distillate sample solution 1 μ l, measures for 5 times according to above-mentioned chromatographic condition continuous sample introduction,Calculate the retention time of 8 chromatographic peaks and the relative standard deviation of peak area (RSD). The RSD of result relative retention time is0.01%～0.22%, the RSD of relative peak area is 0.3%～1.8%, is all less than 2.0%, shows that instrument precision is good,Result of calculation is in Table 5-6.
Table 5 intensified loquet distillate finger-print precision result of calculation (relative retention time)
Table 6 intensified loquet distillate finger-print precision result of calculation (relative peak area)
Embodiment 4 reappearances are investigated
Get respectively with 6 parts of a collection of intensified loquet distillates, prepare need testing solution according to the method under " 4.3.1.7 " item, according toThe UPLC fingerprint map analyzing condition of setting up is analyzed, and the main chromatographic peak of result intensified loquet distillate carrys out retention time relativelyRSD be 0.03%～0.18%, the RSD of relative peak area is 0.68%～1.77%, is all less than 2.0%; Result of calculation is shown inTable 13-1,13-2. Gained chromatogram is imported to similarity evaluation system, calculate similarity, the phase that result intensified loquet distillate reappearsAll be greater than 0.90 like degree, show that the reappearance of method is good, meet the requirement of finger-print, result of calculation is in Table 6-8.
Table 6 intensified loquet distillate reproducibility of fingerprint result of the test (relative retention time)
Table 7 intensified loquet distillate reproducibility of fingerprint result of the test (relative peak area)
Table Final 8 power loquat dew reproducibility of fingerprint similarity result of calculation
Embodiment 5 study on the stability
Wherein 1 part of intensified loquet distillate need testing solution of getting respectively " 4.6.2 " reappearance investigation lower preparation is put in room temperaturePut, measure respectively at 0h, 2h, 4h, 8h, 12h, 16h, 20h sample introduction, the main chromatographic peak relative retention time of intensified loquet distillateRSD is 0.03%～0.18%, and the RSD of relative peak area is 0.44%～1.53%, is all less than 2.0%; Result of calculation is in Table15-1,15-2. Gained chromatogram is imported to similarity evaluation system, calculate similarity, the phase of result intensified loquet distillate stabilityAll be greater than 0.90 like degree. Show that need testing solution is good at 20 hours internal stabilities, the results are shown in Table 9-11.
Table 9 intensified loquet distillate finger-print stability test result (relative retention time)
Table 10 intensified loquet distillate finger-print stability test result (relative peak area)
Table 11 intensified loquet distillate stability similarity result of calculation
Learn checking by said method, fingerprint analysis method precision, reappearance and the stability set up are all goodGood, meet the technical requirement that finger-print is studied, can be used as the quality control standard of intensified loquet distillate.
Claims (8)
1. a method of setting up Sugarless type intensified loquet distillate finger-print, is characterized in that,
It comprises the steps:
The preparation of A need testing solution
B utilizes Ultra Performance Liquid Chromatography instrument, sets up finger-print;
The preparation of test sample comprises the following steps:
1) intensified loquet distillate intermediate: except menthol, the Six-element medicinal material boilings twice such as all the other loguat leaves, each 2h, closesAnd decocting liquid, filtering, filtrate is concentrated into about 750ml, obtains intensified loquet distillate intermediate;
2) preparation of intensified loquet distillate test sample: except menthol, the Six-element medicinal material boilings twice such as all the other loguat leaves, each2h, collecting decoction, filters, and filtrate is concentrated into about 750ml, adds Sodium Benzoate 2.5g, is stirred to dissolve, and adds Steviosin 2g, continuesBe heated to boil, keep 20 minutes, leave standstill, filter, add citric acid 0.5g, the appropriate and menthol of the essence that dissolves with ethanol, stirs,Evenly, leave standstill, filter, add water to 1000ml, mix, obtain intensified loquet distillate sample;
3) test sample of loguat leaf, the tuber of stemona, Cynanchum glaucescens, the root bark of white mulberry and balloonflower root medicinal material be prepared as respectively by loguat leaf, the tuber of stemona, Cynanchum glaucescens,The root bark of white mulberry and balloonflower root medicinal material boiling twice, each 2h, collecting decoction, filters, and filtrate is concentrated, makes respectively loguat leaf, hundredThe simple decocting liquid of portion, Cynanchum glaucescens, the root bark of white mulberry and balloonflower root.
2. the method for building up of finger-print according to claim 1, is characterized in that, the preparation of test sample also comprises followingStep:
The preparation of object of reference solution: it is appropriate that precision takes Sodium Benzoate reference substance, adds methyl alcohol and is mixed with every 1ml and contains Sodium BenzoateThe object of reference solution of 0.2mg;
The preparation of need testing solution: get respectively intensified loquet distillate sample, intensified loquet distillate intermediate, loguat leaf, the tuber of stemona, Cynanchum glaucescens,The simple decocting liquid of the root bark of white mulberry and balloonflower root carries out respectively centrifugal, and precision measures 1ml, upper in SPE solid phase extraction column(WelchromC18E500mg/6ml), water elution is settled in 5ml volumetric flask, shakes up, and 0.22 μ m miillpore filter filters, and gets continuousFiltrate, respectively intensified loquet distillate sample, intensified loquet distillate intermediate, loguat leaf, the tuber of stemona, Cynanchum glaucescens, the root bark of white mulberry and balloonflower rootSimple reference substance.
3. the method for setting up finger-print according to claim 1, is characterized in that,
Accurate object of reference solution and the need testing solution 1 μ l of drawing, injects Ultra Performance Liquid Chromatography instrument respectively, application ACQUITYUPLCBEHC18(2.1 × 100mm, m) chromatographic column of 1.7 μ; Set up finger-print according to UPLC chromatography, record chromatogram, to obtain final productThe chromatogram of corresponding solution to be measured.
4. the method for building up of finger-print according to claim 3, is characterized in that,
Mobile phase application methyl alcohol-0.1% formic acid system wash-out column temperature is 35 DEG C; Flow velocity is 0.3ml/min.
5. the method for building up of finger-print according to claim 3, is characterized in that, detection wavelength is 254nm.
6. the method for building up of finger-print according to claim 3, is characterized in that, similar by chromatographic fingerprints of Chinese materia medicaDegree evaluation system, test sample finger-print and comparison film finger-print calculate through similarity, and similarity must not be lower than 0.90.
7. the method for building up of finger-print according to claim 3, is characterized in that, wherein the program of gradient elution is pressedStating volume by volume concentration configuration carries out: taking methyl alcohol as mobile phase A, 0.1% formic acid is Mobile phase B,
8. the method for building up of Sugarless type intensified loquet distillate finger-print according to claim 3, is characterized in that: described fingerIn line collection of illustrative plates, there is the average retention time at the total peak of feature to comprise, 1.264,2.161,4.539,7.373,12.281.
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