CN106053696A - Method for identifying plant source of herbal rabdosia lophanthide - Google Patents
Method for identifying plant source of herbal rabdosia lophanthide Download PDFInfo
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- CN106053696A CN106053696A CN201610488797.3A CN201610488797A CN106053696A CN 106053696 A CN106053696 A CN 106053696A CN 201610488797 A CN201610488797 A CN 201610488797A CN 106053696 A CN106053696 A CN 106053696A
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- G—PHYSICS
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
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Abstract
The invention provides a method for identifying a plant source of herbal rabdosia lophanthide. The method is based on the high performance liquid chromatography. The method comprises the following steps: using rosmarinic acid, rabdosia lophanthoides apiin A, oridonin, pedalitin and caffeoyl acetate as reference substances; comparing chromatograms of a solution to be tested and a solution mixed with the reference substances, detecting an absorption peak of rosmarinic acid, oridonin and pedalitin under any detection wavelength of 235nm to 240nm and the absorption peak of rosmarinic acid and pedalitin under the detection wavelength of 330nm, and determining the substance to be tested is the plant rabdosia lophanthide; and detecting the absorption peak of rosmarinic acid, rabdosia lophanthoides apiin A and caffeoyl acetate under any detection wavelength of 235nm to 240nm, detecting the absorption peak of rosmarinic acid and caffeoyl acetate under the detection wavelength of 330nm, determining the substance to be tested to be the plant rabdosia lophanthoides or the rabdosia lophanthoides. The method has the advantages of simplicity and convenience in operation, good characteristics, good reproducibility, short time and the like.
Description
Technical field
The invention belongs to the pharmacognosy and analytical chemistry field, be specifically related to a kind of based on high performance liquid chromatography discriminating medical material
The method of the plant origin of Herba Rabdosiae Lophanthoidis.
Background technology
Medical material Herba Rabdosiae Lophanthoidis, for conventional medical herbs among the people, at the other humidity of small stream of happiness raw mountain valley, fresh blade has rubbed yellow juice
And gain the name.Its mildly bitter flavor, cool in nature, have heat clearing away, wet, effect of promoting the function of the gallbladder to alleviate jaundice, be used for treating damp-heat dysentery, traumatic injury congestive edema, urgency
Property icterohepatitis and acute cholecystitis and other.It is special that XIAOYAN LIDAN PIAN with Herba Rabdosiae Lophanthoidis as main material production has become liver and gall
The Chinese patent medicine of sales volume first in section's medication.
For ensuring drug quality, prior art has had been built up the method for qualitative and quantitative detection of some medical material Herba Rabdosiae Lophanthoidiss.
Chinese invention patent application " a kind of medical material Herba Rabdosiae Lophanthoidis such as publication number CN 103399120 A (publication date on November 20th, 2013)
Thin-layer identification method ", disclose using petroleum ether-ethyl acetate (9:1～8:2) as developing solvent, with standard on silica gel plate
Control medicinal material is comparison, and the Herba Rabdosiae Lophanthoidis sample of separate sources is carried out thin-layer developing, mirror method for distinguishing.
But the plant origin of medical material Herba Rabdosiae Lophanthoidis is the most chaotic.Deng Qiaohua etc. report, the Herba Rabdosiae Lophanthoidis on The Qingping Free Market, Guangzhou
Not lower ten several plant sources (Deng Qiaohua, Wang Deqin etc. Herba Rabdosiae Lophanthoidis textual criticism and the checking [J] of character identification method. modern Chinese medicine grinds
Study carefully and put into practice .2014,28 (2): 15-19).It is lip that version " Chinese Pharmacopoeia " annex III in 2010 records the base of Herba Rabdosiae Lophanthoidis first
Section Rabdosia plant Rabdosia lophanthoides Isodon lophanthoides or Herba Rabdosiae Lophanthoidis Isodon sorra (Maxim.) Kudo
(sorra is suspected of serra by mistake).It practice, the various plants of Labiatae Rabdosia, such as Rabdosia lophanthoides Isodon
Lophanthoides and mutation thereof: carefully spend Rabdosia lophanthoides (XIANHUA Rabdosia lophanthoides) Isodon lophanthoides
Var.graciliflora and isodon lophanthoides Isodon Iophanthoides var.gerardianus (Benth.)
H.Hara etc. make medical material Herba Rabdosiae Lophanthoidis and use.
Although Herba Rabdosiae Lophanthoidis Isodon serra (Maxim.) Kudo is of the same name with medical material Herba Rabdosiae Lophanthoidis for plant, pharmacopeia is also classified as
One of base of medical material；But at aspects such as medical material nature and flavor, plant Herba Rabdosiae Lophanthoidis Isodonserra with belong to be used as its of Herba Rabdosiae Lophanthoidis together
All there is the biggest difference in its plant.Specifically:
(1) yellow juice feature
Rabdosia lophanthoides and thin fragrance of a flower tea fresh and being soaked in water to moistening dry blade, has pale brown after rubbing with hands
Color juice, the yellow finger of dye；Plant Herba Rabdosiae Lophanthoidis fresh and being soaked in water to moistening dry blade, the most pale brown after rubbing with hands
Color juice, does not contaminate yellow finger.
(2) nature and flavor feature
Rabdosia lophanthoides and thin flower Rabdosia lophanthoides, sweet-bitter flavor, cool in nature, among the people commonly referred to as " Tian Xihuang ".Plant small stream is yellow
Grass taste is the most bitter, cold in nature, referred to as " bitter small stream is yellow " among the people.
In addition to above-mentioned difference, Deng Qiaohua etc. also finds that the character identification feature of plant Herba Rabdosiae Lophanthoidis with Rabdosia lophanthoides and is carefully spent
Rabdosia lophanthoides is the most dramatically different, does not also correspond with tradition Herba Rabdosiae Lophanthoidis experience diagnostic characteristics；It is taken as that whether plant Herba Rabdosiae Lophanthoidis
Must be able to discuss as medical material Herba Rabdosiae Lophanthoidis use value (Deng Qiaohua, Wang Deqin etc. Herba Rabdosiae Lophanthoidis textual criticism and the checking of character identification method
[J]. R&D of modern TCM with put into practice .2014,28 (2): 15-19).
In order to plant Herba Rabdosiae Lophanthoidis (bitter small stream is yellow) is differentiated with other congener (Tian Xihuang) doing Herba Rabdosiae Lophanthoidis, existing
Technology occurs in that the Chinese invention patent application of entitled " foundation of Herba Rabdosiae Lophanthoidis HPLC-FPS and finger printing thereof "
(publication number 103776926A, publication date on May 7th, 2014), this patent document records the high-efficient liquid phase color yellow with 12 batches of bitter small streams
Based on spectrogram, with caffeic acid, 6-C-arabopyranose base-8-C-glucopyranosyl apigenin, apigenin-8-C-glucoside and Herba Rosmarini Officinalis
Acid is reference substance, with rosmarinic acid absworption peak for reference to peak, establishing the finger printing that bitter small stream is yellow.The document also discloses coffee
Acid, 6-C-arabopyranose base-8-C-glucopyranosyl apigenin, apigenin-8-C-glucoside and rosmarinic acid be Rabdosia lophanthoides,
The chromatographic peak that isodon lophanthoides and XIANHUA Rabdosia lophanthoides have, and plant Herba Rabdosiae Lophanthoidis only has caffeic acid and rosmarinic acid
Peak；Accordingly, plant Herba Rabdosiae Lophanthoidis (bitter small stream is yellow) and other medical material Herba Rabdosiae Lophanthoidis originating species can be distinguished.
The method that above-mentioned discriminating hardship small stream is yellow, in place of Shortcomings:
1) analyze the overlong time of a sample, need 100～120 minutes.
2) discussion is also needed in the selection of reference substance.Caffeic acid is widely present in plant, and its characteristic and representativeness are not dashed forward
Go out.It addition, Tanghai is bright etc., to use HPLC method to measure in separate sources Herba Rabdosiae Lophanthoidis medical material 8 water soluble ingredients (caffeic acid, new simultaneously
The blue apigenin-8-C-glucoside 2 in west, puriri glycosides 3, Isoschaftoside, Schaftoside, apigenin-8-C-glucoside, apigenin-6,8-two-C-α-
L-arabopyranose glycosides and rutin) content, 6 kinds of plant Herba Rabdosiae Lophanthoidiss that result difference commercial channel is buied, have 3 to measure
Apigenin-8-C-glucoside, account for institute test sample product 50% (Tanghai is bright, Chen Jiannan etc., and .HPLC method measures simultaneously in separate sources Herba Rabdosiae Lophanthoidis medical material 8
Individual water soluble ingredient [J]. pharmaceutical analysis magazine .2015,35 (2): 228-234).Therefore, using apigenin-8-C-glucoside as Rabdosia lophanthoides,
Isodon lophanthoides and XIANHUA Rabdosia lophanthoides are different from the feature comparison product of plant Herba Rabdosiae Lophanthoidis, are the most rigorous.
3) finger printing need to carry out Similarity Measure by " similarity evaluation ", to coupling
Degree requires height.Owing to Herba Rabdosiae Lophanthoidis medicinal ingredient is complicated, of a great variety, add that analysis time is longer, chromatographic condition any trickle
Change, can mean that monolithic chromatogram figure makes a variation, it is impossible to match with reference fingerprint, cause erroneous judgement, make to appraisal
Become difficulty, cause the repeatability of experiment to be affected.
Therefore, it is necessary to set up more rigorous, fast and convenient method, with differentiate and distinguish bitter small stream yellow (plant Herba Rabdosiae Lophanthoidis) and
Sweet small stream is yellow (mainly Rabdosia lophanthoides, XIANHUA Rabdosia lophanthoides).
Summary of the invention
For the problems referred to above, it is an object of the present invention to provide a kind of discriminating medical material Herba Rabdosiae Lophanthoidis and derive from plant small stream Huang
Grass, is also derived from the method that plant carefully spends Rabdosia lophanthoides or Rabdosia lophanthoides.The method, based on HPLC method, completes a sample
Product examine is surveyed only needs 50 minutes.
In order to realize reaching above-mentioned technique effect, present invention employs following technical scheme:
A kind of method of plant origin differentiating medical material Herba Rabdosiae Lophanthoidis, described method is based on high performance liquid chromatography, with fan repeatedly
Fragrant colored Rabdosia lophanthoides glycosides A sour, thin, rubescensine A, linum element and caffeic acetate are reference substance, and chromatographic condition includes:
Fixing phase: 18 silane group silica gel；
Flowing phase: with acetonitrile for A phase, concentration of volume percent 0.08～0.3% phosphate aqueous solution be B phase, according to such as
Lower program gradient elution:
It is 18% that 0min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 23% that 33min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 30% that 45min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 34% that 50min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
Flow velocity: 0.6～1.2mL/min；
Column temperature: 23～28 DEG C；
Detection wavelength: the arbitrary wavelength in 235～240nm and 330nm.
Preferably, described B phase is the phosphate aqueous solution of concentration of volume percent 0.1%.
Preferably, described flow velocity is 0.8ml/min.
Preferably, described column temperature is 25 DEG C.
The method of the invention, including the preparation of mixing reference substance solution；Concrete operations are: precision weigh rosmarinic acid,
Thin flower Rabdosia lophanthoides glycosides A, rubescensine A, linum element and caffeic acetate's reference substance, add 50% ethanol and be configured to every 1mL and contain
Rosmarinic acid 20～40 μ g, thin flower Rabdosia lophanthoides glycosides A2～10 μ g, rubescensine A 2～16 μ g, linum element 10～20 μ g, coffee
The mixing reference substance solution of coffee acetoacetic ester 10～25 μ g, to obtain final product.
Said method also includes the preparation of need testing solution；Concrete operations are: weigh dry plant sample powder to be measured,
It is placed in tool plug container, adds 20mL 50% ethanol, close plug, weighed weight, supersound extraction 30min, let cool, the amount of being re-weighed, use
The weight of less loss supplied by 50% ethanol, and 0.22 μm filter membrane filters, takes subsequent filtrate, to obtain final product.
Method of the present invention, also includes determination step；Concrete operations are: the described mixing that accurate absorption prepares
Reference substance solution and need testing solution, be injected separately into high performance chromatograph, under above-mentioned chromatographic condition, in record 235～240nm
The liquid chromatogram of 0～50min under arbitrary wavelength and 330nm.
Above-mentioned method, also includes differentiating step；Concrete, need testing solution and the chromatogram ratio mixing reference substance solution
Relatively, rosmarinic acid, rubescensine A and the absworption peak of linum element occur under the arbitrary detection wavelength in 235～240nm,
Occur rosmarinic acid and the absworption peak of linum element under 330nm detection wavelength, then test sample is plant Herba Rabdosiae Lophanthoidis, for " bitter small stream is yellow "；
Rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A and the suction of caffeic acetate occur under the arbitrary detection wavelength in 235～240nm
Receive peak, occur the absworption peak of rosmarinic acid and caffeic acetate under 330nm detection wavelength, then test sample is plant strain line scented tea
Dish or carefully spend Rabdosia lophanthoides, for " Tian Xihuang ".
As a preferred embodiment, the present invention provide a kind of plant Rabdosia lophanthoides, thin flower Rabdosia lophanthoides and
The discrimination method of plant Herba Rabdosiae Lophanthoidis, described method based on high performance liquid chromatography, with rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A,
Rubescensine A, linum element and caffeic acetate are reference substance, including foundation, the system of mixing reference substance solution of chromatographic condition
Standby, the preparation of need testing solution, measure and differentiate；Concrete operations are:
I. the foundation of chromatographic condition
Fixing phase: 18 silane group silica gel；
Flowing phase: with acetonitrile for A phase, the phosphate aqueous solution of concentration of volume percent 0.1% is B phase, according to following program
Gradient elution:
It is 18% that 0min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 23% that 33min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 30% that 45min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 34% that 50min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
Flow velocity: 0.8ml/min；
Column temperature: 25 DEG C；
Detection wavelength: the arbitrary wavelength in 235～240nm and 330nm；
II. the preparation of reference substance solution is mixed
Precision weighs rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A, rubescensine A, linum element and caffeic acetate's comparison
Product, add 50% ethanol and are configured to every 1mL containing rosmarinic acid 20～40 μ g, thin flower Rabdosia lophanthoides glycosides A 2～10 μ g, Rabdosia rubescens first
Element 2～16 μ g, linum element 10～20 μ g, the mixing reference substance solution of caffeic acetate 10～25 μ g, to obtain final product；
III. the preparation of need testing solution
Weigh dry plant sample powder to be measured, be placed in tool plug container, addition 20mL50% ethanol, close plug, weighed
Weight, supersound extraction 30min, let cool, the amount of being re-weighed, supply the weight of less loss with 50% ethanol, 0.22 μm filter membrane filters, takes continuous
Filtrate, to obtain final product；
IV. measure
It is described for examination that described mixing reference substance solution that accurate aspiration step II prepares and step III prepare
Product solution 10 μ l, is injected separately into high performance chromatograph, under described chromatographic condition, record 235～240nm in arbitrary wavelength and
The liquid chromatogram of 0～50min under 330nm；
V. differentiate
Need testing solution chromatogram step IV obtained compares with the chromatogram of mixing reference substance solution, 235～
Rosmarinic acid, rubescensine A and the absworption peak of linum element occur under the arbitrary detection wavelength in 240nm, detects ripple at 330nm
Occur rosmarinic acid and the absworption peak of linum element under length, then test sample is plant Herba Rabdosiae Lophanthoidis (bitter small stream is yellow)；In 235～240nm
Arbitrary detection wavelength under rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A and the absworption peak of caffeic acetate occur, examine at 330nm
Survey the absworption peak occurring rosmarinic acid and caffeic acetate under wavelength, then test sample is plant Rabdosia lophanthoides or thin yarn stricture of vagina perfume
Tea dish (Tian Xihuang).
In the method for the invention, when preparing need testing solution, plant sample to be measured was the powder of 60 mesh.
In description of the invention, not having specified otherwise, " Herba Rabdosiae Lophanthoidis " refers to medical material Herba Rabdosiae Lophanthoidis；" bitter small stream is yellow " refers to plant
Thing Herba Rabdosiae Lophanthoidis；" Tian Xihuang " refers to Rabdosia lophanthoides and/or carefully spends Rabdosia lophanthoides.
In description of the invention, " 50% ethanol " refers to ethanol concentration of volume percent is 50%, typically measures with ethanol
Fixed.
Inventor is through further investigation and has carried out substantial amounts of experiment, finds: Rabdosia lophanthoides, thin flower Rabdosia lophanthoides etc.
Containing rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A, 3 kinds of compositions of caffeic acetate, and Herba Rabdosiae Lophanthoidis without thin flower Rabdosia lophanthoides glycosides A,
2 kinds of compositions of caffeic acetate；Plant Herba Rabdosiae Lophanthoidis is containing rosmarinic acid, rubescensine A, linum three kinds of compositions of element, and strain line scented tea
Dish, thin flower Rabdosia lophanthoides are without rubescensine A, linum 2 kinds of compositions of element, therefore with rosmarinic acid, thin flower Rabdosia lophanthoides glycosides
A, caffeic acetate, rubescensine A and linum element are reference substance, and characteristic is strong, according to the feature occurred in HPLC-UV detection
Become subassembly, it is possible to identify whether medical material derives from plant Herba Rabdosiae Lophanthoidis.
Accompanying drawing explanation
Hereinafter, describe embodiment of the present invention in detail in conjunction with accompanying drawing, wherein:
Fig. 1 is the high-efficient liquid phase chromatogram of the mixing reference substance that embodiment 1 obtains, the chromatogram under wherein 1A is 240nm,
1B is the chromatogram under 330nm；In figure, No. 1 peak is the absworption peak of rosmarinic acid, and No. 2 peaks are the suction carefully spending Rabdosia lophanthoides glycosides A
Receiving peak, No. 3 peaks are the absworption peak of rubescensine A, and No. 4 peaks are the absworption peak of linum element, and No. 5 peaks are the absorption of caffeic acetate
Peak.
Fig. 2 is the high-efficient liquid phase chromatogram of the plant Herba Rabdosiae Lophanthoidis that embodiment 2 obtains, the chromatogram under wherein 2A is 240nm,
2B is the chromatogram under 330nm；In figure, No. 1 peak is the absworption peak of rosmarinic acid, and No. 2 peaks are the suction carefully spending Rabdosia lophanthoides glycosides A
Receiving peak, No. 3 peaks are the absworption peak of rubescensine A, and No. 4 peaks are the absworption peak of linum element, and No. 5 peaks are the absorption of caffeic acetate
Peak.
Fig. 3 is the high-efficient liquid phase chromatogram of the strain line scented tea that embodiment 3 obtains, the chromatogram under wherein 3A is 240nm, 3B
It it is the chromatogram under 330nm；In figure, No. 1 peak is the absworption peak of rosmarinic acid, and No. 2 peaks are the absorption carefully spending Rabdosia lophanthoides glycosides A
Peak, No. 3 peaks are the absworption peak of rubescensine A, and No. 4 peaks are the absworption peak of linum element, and No. 5 peaks are the absworption peak of caffeic acetate.
Fig. 4 is the high-efficient liquid phase chromatogram of the thin yarn stricture of vagina scented tea that embodiment 4 obtains, the chromatograph under wherein 4A is 240nm
Figure, 4B is the chromatogram under 330nm；In figure, No. 1 peak is the absworption peak of rosmarinic acid, and No. 2 peaks are carefully to spend Rabdosia lophanthoides glycosides A
Absworption peak, No. 3 peaks are the absworption peak of rubescensine A, and No. 4 peaks are the absworption peak of linum element, and No. 5 peaks are the suction of caffeic acetate
Receive peak.
Fig. 5 is the high-efficient liquid phase chromatogram of 10 batch samples (S1～S10), the color of sample S1～S5 under wherein 5A is 235nm
Spectrogram, 5B is the chromatogram of sample S6～S10 under 235nm, and 5C is the chromatogram of sample S1～S5 under 330nm, and 5D is under 330nm
The chromatogram of sample S6～S10；In figure, No. 1 peak is the absworption peak of rosmarinic acid, and No. 2 peaks are the suction carefully spending Rabdosia lophanthoides glycosides A
Receiving peak, No. 3 peaks are the absworption peak of rubescensine A, and No. 4 peaks are the absworption peak of linum element, and No. 5 peaks are the absorption of caffeic acetate
Peak.
Detailed description of the invention
Referring to specific embodiment, the present invention is described.Only it will be appreciated by those skilled in the art that these embodiments
For the present invention is described, it limits the scope of the present invention never in any form.
Experimental technique in following embodiment, if no special instructions, is conventional method.Medicine used in following embodiment
Material raw material, reagent material etc., if no special instructions, be commercially available purchase product.
Instrument, reagent and medical material used in following example and source thereof be:
1. instrument
Agilent 1260 type high performance liquid chromatograph, including Chemstation chromatographic work station, the detection of G1314B type DAD
Device, G1311C type quaternary pump, G1329B type automatic sampler, G1316A type column oven (Agilent company of the U.S.)；
AgiLent EcLipse XDB-C18(4.6mm × 250mm, 5 μm) chromatographic column；
BT125D type 100,000/electronic balance (Sartorius AG)；
Ultrasonic cleaner (Kunshan Shu Mei ultrasonic instrument company limited, model: KQ-300VDE, power: 300KW, frequency:
45KHz)。
2. reagent
95% ethanol (analytical pure) specification: 500mL, Guangzhou Jia Le Chemical Co., Ltd.；
Deionized water, self-control.
3. reference substance:
Rosmarinic acid (lot number: 111871-201404, National Institute for Food and Drugs Control), thin flower Rabdosia lophanthoides glycosides A
(lot number: 20160226, laboratory is made by oneself, detects purity ＞ 98.0% through HPLC), rubescensine A (lot number: 111721-
201403, National Institute for Food and Drugs Control), linum element (lot number: BBP02771, ethylmercuric cloride thing Science and Technology Ltd., purity
＞ 98.0%) and caffeic acetate's (lot number: 20160228, laboratory is made by oneself, detects purity ＞ 98.0% through HPLC).
4. treat measuring plants
Rabdosia lophanthoides, flower Rabdosia lophanthoides, be purchased from Ge great pharmacy or adopt in Qingyuan City, Germany and Britain, multiple GAP kinds such as Fujian are planted
Base, identifies through South China Botanical Garden Ye Huagu researcher and is respectively Rabdosia lophanthoides Isodon lophanthoides, thin yarn
The dry aerial parts of stricture of vagina Herba Rabdosiae glaucocalycis (XIANHUA Herba Rabdosiae glaucocalycis) Isodon lophanthoides var.graciliflora.
Herba Rabdosiae Lophanthoidis, be purchased from Ge great pharmacy or adopt in Qingyuan City, Germany and Britain, multiple GAP planting bases such as Fujian, through South China Botanical Garden
Ye Huagu researcher identifies and is respectively Herba Rabdosiae Lophanthoidis Isodon serra (Maxim.) Kudo dry aerial parts.
Embodiment 1The foundation of reference substance high-efficient liquid phase chromatogram
1. chromatographic condition:
Chromatographic column: AgiLent EcLipse XDB-C18(4.6mm × 250mm, 5 μm) chromatographic column.
Flowing phase: be A phase with acetonitrile, with percent by volume be 0.08～the phosphate aqueous solution of 0.3% carries out gradient for B phase
Eluting.When test finds the phosphate aqueous solution that B phase is 0.1% (vol%), the absworption peak peak shape of each reference substance is good, separating degree
Height, baseline is steady, and therefore B phase is preferably the phosphate aqueous solution of 0.1% (vol%).Eluent gradient elution requirement is shown in Table 1.
Table 1 gradient elution program
Flow velocity: 0.6～1.2mL/min；Through test, find that during flow velocity 0.8mL/min, separating effect is best, the most preferably flows
Speed is 0.8mL/min.
Column temperature: 23～28 DEG C, preferably 25 DEG C.
Ultraviolet detection wavelength: recall rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A, rubescensine A, linum element, coffee respectively
The long chromatogram of liquid phase DAD all-wave of 5 kinds of compositions of coffee acetoacetic ester, result rosmarinic acid, linum element, the absorption maximum of caffeic acetate
Wavelength is 330nm, and a length of 235nm of maximum absorption wave of thin flower Rabdosia lophanthoides glycosides A, the maximum absorption wave of rubescensine A is a length of
238nm.Comprehensively examine filter, the arbitrary wavelength in 235～240nm and 330nm dual wavelength can be used to be measured, can measure simultaneously
Rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A, rubescensine A, linum element, 5 kinds of compositions of caffeic acetate.The present embodiment uses
240nm and 330nm dual wavelength is measured
Elution time: 50min.
2. the preparation of mixing reference substance solution:
The present invention mixes reference substance and can be prepared via a method which: precision weighs rosmarinic acid, carefully spends Rabdosia lophanthoides
Glycosides A, rubescensine A, linum element and caffeic acetate's reference substance are appropriate, add 50% ethanol and are configured to every 1mL containing rosmarinic acid 20
～40 μ g, thin flower Rabdosia lophanthoides glycosides A 2～10 μ g, rubescensine A 2～16 μ g, linum element 10～20 μ g, caffeic acetate
The mixing reference substance solution of 10～25 μ g, to obtain final product.
Specific to the present embodiment, mixing reference substance solution is prepared via a method which:
Precision weighs rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A, rubescensine A, linum element and caffeic acetate's comparison
Product are respectively 6.49,2.28,4.06,3.32,4.09mg, be respectively placed in the molten measuring bottle of 10mL, add 50% ethanol and be configured to respectively
Every 1mL is containing rosmarinic acid 649.0 μ g, thin flower Rabdosia lophanthoides glycosides A 228.0 μ g, rubescensine A 406.0 μ g, linum element
The single reference substance storing solution of 331.6 μ g and caffeic acetate 409.0 μ g, take respectively single reference substance solution 0.5,0.2,0.2,
0.5, during 0.5mL is placed in 10mL volumetric flask, add 50% ethanol constant volume, be made into every 1mL containing rosmarinic acid 32.45 μ g, thin yarn stricture of vagina
Herba Rabdosiae glaucocalycis glycosides A 4.56 μ g, rubescensine A 8.12 μ g, linum element 16.58 μ g, the mixing reference substance of caffeic acetate 20.45 μ g
Solution.
3. measure:
Accurate draw described mixing reference substance solution 10 μ l, inject high performance liquid chromatograph, under record 240nm and 330nm 0
～the chromatogram of 50min, it is specifically shown in Fig. 1.It will be seen from figure 1 that each reference substance separating degree is good, the most substantially do not interfere with.Especially
It is carefully to spend Rabdosia lophanthoides glycosides A and rubescensine A, has basically reached baseline separation.Illustrate the chromatographic condition of the present invention for
The separation of above-mentioned mixing reference substance is applicable.
The absworption peak of rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A, rubescensine A, linum element and caffeic acetate is respectively
It is numbered 1～5.240nm and 330nm detection wavelength under, each reference substance go out peak situation and retention time, be shown in Table 2.
Table 2 reference substance go out peak situation
| Retention time (min) | 240nm330nm | |
| Rosmarinic acid | 26.863±0.100 | +a+a |
| Thin flower Rabdosia lophanthoides glycosides A | 30.063±0.100 | +a+a |
| Rubescensine A | 30.770±0.100 | +a-b |
| Linum element | 33.891±0.100 | +a+a |
| Caffeic acetate | 39.761±0.100 | +a+a |
a: represent and absworption peak detected；b: represent and be not detected by absworption peak
Embodiment 2The high-efficient liquid phase chromatogram of plant Herba Rabdosiae Lophanthoidis is set up
1. chromatographic condition
With the preferred chromatographic condition of embodiment 1, wherein ultraviolet detection wavelength is 240nm and 330nm.
2. mix the preparation of reference substance solution
" preparation of mixing reference substance solution " with embodiment 1.
3. the preparation of need testing solution
Weigh dry plant Herba Rabdosiae Lophanthoidis powder 0.5g, accurately weighed, it is placed in tool plug triangular flask, adds 20mL50% second
Alcohol, close plug, weighed weight, supersound extraction 30min, let cool, the amount of being re-weighed, supply the weight of less loss, 0.22 μm with 50% ethanol
Filter membrane filters, and takes subsequent filtrate, to obtain final product.
4. measure
Described mixing reference substance solution that accurate aspiration step 2 prepares and the described test sample that step 3 prepares
Solution 10 μ l, is injected separately into high performance chromatograph, under described chromatographic condition, and the liquid phase of 0～50min under record 240nm and 330nm
Chromatogram, is specifically shown in Fig. 2.
Comparing with the chromatogram of mixing reference substance solution, judge according to the retention time of absworption peak, plant Herba Rabdosiae Lophanthoidis exists
Occur in that rosmarinic acid, rubescensine A and the absworption peak of linum element under 240nm, under 330nm, the most only occur in that rosmarinic acid
Absworption peak with linum element.
Embodiment 3The high-efficient liquid phase chromatogram of Rabdosia lophanthoides is set up
1. chromatographic condition
With the preferred chromatographic condition of embodiment 1, wherein ultraviolet detection wavelength is 240nm and 330nm.
2. mix the preparation of reference substance solution
" preparation of mixing reference substance solution " with embodiment 1.
3. the preparation of need testing solution
Weigh dry Rabdosia lophanthoides powder 0.5g, accurately weighed, it is placed in tool plug triangular flask, adds 20mL50% second
Alcohol, close plug, weighed weight, supersound extraction 30min, let cool, the amount of being re-weighed, supply the weight of less loss, 0.22 μm with 50% ethanol
Filter membrane filters, and takes subsequent filtrate, to obtain final product.
4. measure
Described mixing reference substance solution that accurate aspiration step 2 prepares and the described test sample that step 3 prepares
Solution 10 μ l, is injected separately into high performance chromatograph, under described chromatographic condition, and the liquid phase of 0～50min under record 240nm and 330nm
Chromatogram, is specifically shown in Fig. 3.
Compare with the chromatogram of mixing reference substance solution, judge according to the retention time of absworption peak, plant Rabdosia lophanthoides
Under 240nm, occur in that rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A and the absworption peak of caffeic acetate, the most only go out under 330nm
Show the absworption peak of rosmarinic acid and caffeic acetate.
Embodiment 4The high-efficient liquid phase chromatogram of thin flower Rabdosia lophanthoides is set up
1. chromatographic condition
With the preferred chromatographic condition of embodiment 1, wherein ultraviolet detection wavelength is 240nm and 330nm.
2. mix the preparation of reference substance solution
" preparation of mixing reference substance solution " with embodiment 1.
3. the preparation of need testing solution
Weigh dry thin flower Rabdosia lophanthoides powder 0.5g, accurately weighed, it is placed in tool plug triangular flask, adds
20mL50% ethanol, close plug, weighed weight, supersound extraction 30min, let cool, the amount of being re-weighed, supply the weight of less loss with 50% ethanol
Amount, 0.22 μm filter membrane filters, takes subsequent filtrate, to obtain final product.
4. measure
Described mixing reference substance solution that accurate aspiration step 2 prepares and the described test sample that step 3 prepares
Solution 10 μ l, is injected separately into high performance chromatograph, under described chromatographic condition, and the liquid phase of 0～50min under record 240nm and 330nm
Chromatogram, is specifically shown in Fig. 3.
Comparing with the chromatogram of mixing reference substance solution, judge according to the retention time of absworption peak, plant thin yarn stricture of vagina is fragrant
Tea dish occurs in that rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A and the absworption peak of caffeic acetate under 240nm, under 330nm then
Only occur in that the absworption peak of rosmarinic acid and caffeic acetate.
The result of above-described embodiment 2～4 shows, plant Herba Rabdosiae Lophanthoidis and Rabdosia lophanthoides, thin flower Rabdosia lophanthoides are at this
Chromatogram under bright described chromatographic condition has dramatically different feature, can differentiate rapidly accordingly to use as Herba Rabdosiae Lophanthoidis
The source of plant.
Embodiment 5The plant-origin of medical material Herba Rabdosiae Lophanthoidis differentiates
Collect medical material Herba Rabdosiae Lophanthoidis 10 parts from different channels, identify, really through character (yellow juice, plant outward appearance and micro-character)
Its plant-origin fixed, is specifically shown in Table 3.Above-mentioned medical material Herba Rabdosiae Lophanthoidis is transferred to analyzes laboratory technician's random number and (does not inform its plant base
Former), respectively according to the method and steps (but, wherein ultraviolet detection wavelength is 235nm and 330nm) of embodiment 3, mixed
Reference substance and each sample 235nm and the chromatogram of 330nm.
The chromatogram of each sample is compared with the mixing corresponding chromatogram of reference substance, goes out the situation at peak according to reference substance, sentence
Disconnected sample is " bitter small stream is yellow " (plant Herba Rabdosiae Lophanthoidis), or " Tian Xihuang " (thin flower Rabdosia lophanthoides or Rabdosia lophanthoides).Result is shown in
Table 3.
Table 3 medical material Herba Rabdosiae Lophanthoidis plant-origin identification result
From table 3 it can be seen that utilize the method for the present invention to differentiate the plant-origin of medical material Herba Rabdosiae Lophanthoidis, result and classical property
Shape phase demodulation meets, and can differentiate that medical material Herba Rabdosiae Lophanthoidis is " bitter small stream is yellow " or " Tian Xihuang " rapidly.
Specific description of embodiments of the present invention above is not limiting as the present invention, and those skilled in the art can be according to this
Various change or deformation are made in invention, without departing from the spirit of the present invention, all should belong to the model of claims of the present invention
Enclose.
Claims (10)
1. the method differentiating the plant origin of medical material Herba Rabdosiae Lophanthoidis, described method is based on high performance liquid chromatography, with Herba Rosmarini Officinalis
Colored Rabdosia lophanthoides glycosides A sour, thin, rubescensine A, linum element and caffeic acetate are reference substance, and chromatographic condition includes:
Fixing phase: 18 silane group silica gel；
Flowing phase: with acetonitrile for A phase, concentration of volume percent 0.08～0.3% phosphate aqueous solution be B phase, according to following journey
Sequence gradient elution:
It is 18% that 0min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 23% that 33min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 30% that 45min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 34% that 50min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
Flow velocity: 0.6～1.2mL/min；
Column temperature: 23～28 DEG C；
Detection wavelength: the arbitrary wavelength in 235～240nm and 330nm.
Method the most according to claim 1, it is characterised in that described B phase is the phosphoric acid water of concentration of volume percent 0.1%
Solution.
Method the most according to claim 1, it is characterised in that described flow velocity is 0.8ml/min.
Method the most according to claim 1, it is characterised in that described column temperature is 25 DEG C.
Method the most according to any one of claim 1 to 4, it is characterised in that it is molten that described method includes mixing reference substance
The preparation of liquid；Concrete operations are: precision weighs rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A, rubescensine A, linum element and coffee
Coffee acetoacetic ester reference substance, adds 50% ethanol and is configured to every 1mL containing rosmarinic acid 20～40 μ g, thin flower Rabdosia lophanthoides glycosides A2～10
μ g, rubescensine A 2～16 μ g, linum element 10～20 μ g, the mixing reference substance solution of caffeic acetate 10～25 μ g, to obtain final product.
Method the most according to any one of claim 1 to 5, it is characterised in that described method also includes need testing solution
Preparation；Concrete operations are: weigh dry plant sample powder to be measured, are placed in tool plug container, add 20mL 50% second
Alcohol, close plug, weighed weight, supersound extraction 30min, let cool, the amount of being re-weighed, supply the weight of less loss, 0.22 μm with 50% ethanol
Filter membrane filters, and takes subsequent filtrate, to obtain final product.
Method the most according to any one of claim 1 to 6, it is characterised in that described method, also includes measuring step
Suddenly；Concrete operations are: precision draws the described mixing reference substance solution and need testing solution prepared, and is injected separately into efficient color
Spectrometer, under above-mentioned chromatographic condition, records the liquid chromatograph of 0～50min under the arbitrary wavelength in 235～240nm and 330nm
Figure.
Method the most according to any one of claim 1 to 7, it is characterised in that described method also includes differentiating step；Tool
Body, need testing solution compares with the chromatogram of mixing reference substance solution, goes out under the arbitrary detection wavelength in 235～240nm
Existing rosmarinic acid, rubescensine A and the absworption peak of linum element, occur rosmarinic acid and linum element under 330nm detection wavelength
Absworption peak, then test sample is plant Herba Rabdosiae Lophanthoidis；Under arbitrary detection wavelength in 235～240nm, rosmarinic acid, thin yarn occur
Stricture of vagina Herba Rabdosiae glaucocalycis glycosides A and the absworption peak of caffeic acetate, occur the suction of rosmarinic acid and caffeic acetate under 330nm detection wavelength
Receive peak, then test sample is plant Rabdosia lophanthoides or carefully spends Rabdosia lophanthoides.
9. plant Rabdosia lophanthoides, thin flower Rabdosia lophanthoides and a discrimination method for plant Herba Rabdosiae Lophanthoidis, described method is based on height
Effect liquid phase chromatogram method, with rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A, rubescensine A, linum element and caffeic acetate for comparison
Product, including chromatographic condition foundation, mixing the preparation of reference substance solution, the preparation of need testing solution, measure and differentiate；Concrete behaviour
As:
I. the foundation of chromatographic condition
Fixing phase: 18 silane group silica gel；
Flowing phase: with acetonitrile for A phase, the phosphate aqueous solution of concentration of volume percent 0.1% is B phase, according to following program gradient
Eluting:
It is 18% that 0min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 23% that 33min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 30% that 45min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
It is 34% that 50min, A phase accounts for the percent by volume of flowing phase, and remaining is B phase,
Flow velocity: 0.8ml/min；
Column temperature: 25 DEG C；
Detection wavelength: the arbitrary wavelength in 235～240nm and 330nm；
II. the preparation of reference substance solution is mixed
Precision weighs rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A, rubescensine A, linum element and caffeic acetate's reference substance, adds
50% ethanol be configured to every 1mL containing rosmarinic acid 20～40 μ g, thin flower Rabdosia lophanthoides glycosides A 2～10 μ g, rubescensine A 2～
16 μ g, linum element 10～20 μ g, the mixing reference substance solution of caffeic acetate 10～25 μ g, to obtain final product；
III. the preparation of need testing solution
Weigh dry plant sample powder to be measured, be placed in tool plug container, addition 20mL50% ethanol, close plug, weighed weight,
Supersound extraction 30min, lets cool, the amount of being re-weighed, and supplies the weight of less loss with 50% ethanol, and 0.22 μm filter membrane filters, takes subsequent filtrate,
Obtain；
IV. measure
Described mixing reference substance solution that accurate aspiration step II prepares and the described test sample that step III prepares are molten
Liquid 10 μ l, is injected separately into high performance chromatograph, under described chromatographic condition, and the arbitrary wavelength in record 235～240nm and 330nm
The liquid chromatogram of lower 0～50min；
V. differentiate
Need testing solution chromatogram step IV obtained compares, in 235～240nm with the chromatogram of mixing reference substance solution
Arbitrary detection wavelength under occur rosmarinic acid, rubescensine A and linum element absworption peak, 330nm detection wavelength under occur
Rosmarinic acid and the absworption peak of linum element, then test sample is plant Herba Rabdosiae Lophanthoidis；Under arbitrary detection wavelength in 235～240nm
Rosmarinic acid, thin flower Rabdosia lophanthoides glycosides A and the absworption peak of caffeic acetate occur, under 330nm detection wavelength, occurs that fan is repeatedly
Fragrant acid and the absworption peak of caffeic acetate, then test sample is plant Rabdosia lophanthoides or carefully spends Rabdosia lophanthoides.
Method the most according to any one of claim 1 to 9, it is characterised in that when preparing need testing solution, to be measured plants
Thing sample was the powder of 60 mesh.
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