CN102507830A - High performance liquid chromatograph method for measuring content of Quzhazhigan in Rheum lhasaense - Google Patents
High performance liquid chromatograph method for measuring content of Quzhazhigan in Rheum lhasaense Download PDFInfo
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Abstract
The invention discloses a high performance liquid chromatograph method for measuring the content of Quzhazhigan in Rheum lhasaense. The method takes mixed solution formed by organic solvent and 0.1% phosphoric acid water solution as mobile phase, wherein the volume percentage of organic solvent is 15% to 30% and the volume percentage of 0.1% phosphoric acid water solution is 70% to 85%; the high performance liquid chromatograph is performed to analyze the content of Quzhazhigan in a sample. The method establishes the high performance liquid chromatograph method for measuring the content of Quzhazhigan in Rheum lhasaense for the first time through systematical comparison and study, has the technical characteristics of excellent separation effect, accurate measurement, high specificity, convenience and quickness in analysis and the like, and has direct application value in accurately mastering the change of the active ingredient Quzhazhigan in the product during planting, storing, extracting and processing.
Description
Technical field
The present invention relates to the analytical chemistry field, particularly a kind of efficient liquid-phase chromatography method of measuring Quzhazhigan content in the Lhasa rhubarb.
Background technology
Lhasa rhubarb Rheum lhasaense A.J.Li et P.K.Hsiao is a Rheum ripple leaf group plant.Tibetan's herbal medicine of using among the people is hidden and is named as bent letter, dries with rhizome and is used as medicine.Classify it as " inferior rheum officinale " in " newly repairing brilliant pearl book on Chinese herbal medicine ", promptly commonly use kind for one of " bent letter " medicinal material, its root and rhizome is used as medicine.Say in " Bao Shu complies with one's wishes " " inferior rheum officinale property is slow, and is sharp, and voltinism is flat ".Wild Lhasa rhubarb main product is in China Tibet, Sichuan and other places.Through early-stage Study, we have found the active component Quzhazhigan in the Lhasa rhubarb, have the effect of treatment cerebral arterial thrombosis, and have applied for patent " a kind of Quzhazhigan crystal and preparation method thereof and application ", number of patent application 201110166486.2.Quzhazhigan is compound (E)-1-(3, the 5-dihydroxyphenyl)-2-(3-hydroxyl-4-O-β-D-glucopyranose phenyl) ethene, or becomes 3; 5,3 ', 4 '-tetrahydroxy Stilbene-3 '-O-beta-glucosidase (has again and claims 3; 5,4 '-trihydroxy-Stilbene-3 '-the O-glucoside).Chemical structural drawing is following:
Detection commonly used with separate Lhasa rhubarb in the method for Quzhazhigan comprise high performance liquid chromatography etc.High performance liquid chromatography (High Performance Liquid HPLC) is claimed " high pressure liquid chromatography ", " high-speed liquid chromatography ", " high separation liquid chromatography ", " column chromatography in modern age " etc. again.High performance liquid chromatography is a chromatographic important branch; With liquid is moving phase; Adopt the high pressure transfusion system, the moving phases such as mixed solvent, damping fluid that will have single solvent or the different proportion of opposed polarity pump into the chromatographic column that stationary phase is housed, in post each composition separated after; Get into detecting device and detect, thereby realize analysis sample.
But at present, in utilizing the high performance liquid chromatography detection and separating Lhasa rhubarb, exist some problems and shortcoming in the method for Quzhazhigan.Such as, can't effectively separate, not reach degree of separation with other compositions and require or the like.Through research, these are all relevant with the composition and the ratio of selected moving phase.Therefore, find a kind of suitable use high performance liquid chromatography detect with separates Lhasa rhubarb in the method for Quzhazhigan be that realization utilizes Quzhazhigan to prepare the basis of medicine and suitability for industrialized production.
Summary of the invention
The technical matters that the present invention will solve is the low problem of degree of separation that the HPLC analytical method to Quzhazhigan in the prior art exists, and the method for Quzhazhigan content in a kind of accurate mensuration Lhasa rhubarb is provided.
For solving the problems of the technologies described above, technical scheme provided by the invention is:
A kind of efficient liquid-phase chromatography method of measuring Quzhazhigan content in the Lhasa rhubarb; The mixed solution of forming with organic solvent and 0.1% phosphate aqueous solution is a moving phase; It forms volume content is organic solvent 15%-30%; 0.1% phosphate aqueous solution 70%-85% carries out high performance liquid chromatography, the content of Quzhazhigan in the analytic sample.
High-performance liquid chromatogram determination of the present invention selects for use the most frequently used carbon octadecyl silane post to carry out stratographic analysis.The inventor has also compared the Luna C-18 of Phenomenex company post, the Apollo C-18 of Grace company post, the Cosmosil C-18 of Nacalai Tesque company post etc., and better separating effect is all arranged.
In one embodiment of the invention, the inventor measures ultraviolet spectrum through getting the Quzhazhigan reference substance after with dissolve with methanol, confirms the detection wavelength of high performance liquid chromatography.Experimental result shows, in that the absorption value of 200nm and 216nm is big but near terminal absorption region, the absorption value maximum and the absorption peak at 318.5nm place are more smooth, so the detection wavelength is selected 319nm for use.
According to conventional method, the flow rate of mobile phase of efficient liquid-phase chromatography method of the present invention is selected 1ml/min for use; Chromatogram column temperature is selected 30 ℃ for use; Sampling volume is selected 10ul for use.
In one embodiment of the invention, the inventor has compared different moving phases, and the moving phase of different proportion is to detecting the influence of separating effect.Experimental result shows, under the constant situation of other conditional parameters, with the moving phase that the first alcohol and water is formed according to 40: 60 mixed, Quzhazhigan becomes swarmings to separate bad with other in the test sample; With the moving phase that acetonitrile and water are formed according to 20: 80 mixed, Quzhazhigan becomes swarming to separate bad with other in the test sample; Moving phase so that acetonitrile and 0.1% phosphoric acid solution are formed according to 10: 90 mixed is carried out gradient elution, though Quzhazhigan and other compositions and other component separating in the test sample, degree of separation does not reach requirement; With acetonitrile and 0.1% phosphoric acid solution according to 15: 85, with methyl alcohol and 0.1% phosphoric acid solution according to 30: 70 and with organic solvent and 0.1% phosphoric acid solution according to 15-30: arbitrary proportion mixes the moving phase of forming and carries out gradient elution between the 70-85; Quzhazhigan can effectively separate with other compositions in the test sample, and reaches the degree of separation requirement.Therefore, the composition volume content of organic solvent of the present invention and 0.1% phosphoric acid solution is organic solvent 15%-30%, 0.1% phosphate aqueous solution 70%-85%.
As preferably, organic solvent is the mixed solvent of one or more compositions in acetonitrile, methyl alcohol, ether, normal hexane or the cyclohexane among the present invention.
More preferably, organic solvent is acetonitrile or methyl alcohol among the present invention.
In an embodiment of the present invention, the inventor has carried out the methodology checking to above-mentioned institute selected parameter.Comprising the precision of checking sample introduction, the repeatability of method, the stability of solution, the linearity and the recovery of method.Experimental result shows that the high performance liquid chromatography parameter that the present invention selected for use can satisfy the detection separation requirement to Quzhazhigan in the sample.
In an embodiment of the present invention; The inventor measures the content of Quzhazhigan in the Lhasa rhubarb study sample of different batches; Experimental result shows, in high performance liquid chromatography parameter area of the present invention, the content of Quzhazhigan is same or similar in same batch of study sample.
Major advantage of the present invention is following:
(1) the present invention has set up the efficient liquid-phase chromatography method of measuring Quzhazhigan content in the Lhasa rhubarb first through systematic comparison research;
Technical characterstics such as (2) method among the present invention has good separating effect, measures accurately, and is highly sensitive, and specificity is strong, analytical approach is easy;
(3) method among the present invention plants, stores, extracts the variation of effective constituent Quzhazhigan in the processes such as processing to accurate grasp kind, and direct using value is arranged.
Description of drawings
Fig. 1 is the uv absorption spectra of Quzhazhigan standard specimen in methyl alcohol;
Fig. 2 is the HPLC chromatogram of Quzhazhigan reference substance.
Embodiment
The invention discloses a kind of efficient liquid-phase chromatography method of measuring Quzhazhigan content in the Lhasa rhubarb, those skilled in the art can use for reference this paper content, suitably improve technological parameter and realize.Special needs to be pointed out is that all similarly replace and change apparent to those skilled in the art, they all are regarded as and are included in the present invention.Method of the present invention and application are described through preferred embodiment; The related personnel obviously can change or suitably change and combination methods and applications as herein described in not breaking away from content of the present invention, spirit and scope, realizes and use technology of the present invention.
Principle of work of the present invention and process are that the extract of Lhasa rhubarb medicinal material injects high performance liquid chromatograph; By volume content is organic solvent 15%-30%; The mixed solution that the organic solvent of 0.1% phosphate aqueous solution 70%-85%-0.1% phosphate aqueous solution is formed is that moving phase carries composition entering chromatographic columns such as Quzhazhigan; The chromatographic column that with the carbon octadecyl silane is filling agent is separated Quzhazhigan with other chemical constitutions, make it arrive UV-detector and identification to be detected successively; Detecting device is measured the response at Quzhazhigan peak in the Lhasa rhubarb sample, and respectively corresponding its sample size how much, through the size of its response and the content that relatively calculates Quzhazhigan in the Lhasa rhubarb sample of Quzhazhigan standard specimen.
In order to make those skilled in the art understand technical scheme of the present invention better, the present invention is done further detailed description below in conjunction with specific embodiment.
The instrument that following examples adopted with receive the reagent article:
Instrument: Tianjin, island UV2450 ultraviolet spectrophotometer, wear peace U3000 type liquid chromatograph, plum Teller type analysis balance.
Reagent: the self-control of reference substance Quzhazhigan, lot number 20110308, purity 99% (appraisal basis: specific rotation, ultraviolet spectrum, mass spectrum, hydrogen spectrum, carbon spectrum; The purity test method: HPLC normalization mass concentration is greater than 99%), Lhasa rhubarb medicinal material, lot number 20091027,20100927,20110827.
Embodiment 1: the selection of experimental technique condition and foundation
1, chromatographic column selects for use
Consider the ubiquity of application, select for use HPLC to measure the most frequently used carbon octadecyl silane post.Compared the Luna C-18 of Phenomenex company post, the Apollo C-18 of Grace company post, the Cosmosil C-18 of Nacalai Tesque company post etc., better separating effect has all been arranged.
2, detecting wavelength confirms
Get the Quzhazhigan reference substance and measure ultraviolet spectrum after with dissolve with methanol, the result sees Fig. 1, has ultraviolet absorption curve, and three main absorption bands are arranged.Wherein the absorption value of 200nm and 216nm is big but near terminal absorption region, the absorption value maximum and the absorption peak at 318.5nm place are more smooth, so the detection wavelength is selected 319nm for use.
3, the selection of moving phase
The Lhasa rhubarb complicated component selects suitable moving phase to obtain the key that good separating effect is an analytical approach.Select for use flow phase system such as methanol-water, acetonitrile-water to compare screening, all can't separate the relevant composition in the Lhasa rhubarb fully.Variation tendency according to the major component peak; Moving phase is adjusted into organic solvent-0.1% phosphate aqueous solution; According to volume content is organic solvent 15%-30%; The moving phase that the ratio of 0.1% phosphate aqueous solution 70%-85% is formed is carried out gradient elution, has separating effect preferably, and test findings is seen table 1.
Table 1 moving phase contrast shaker test data
" an appendix VI of Chinese pharmacopoeia D high performance liquid chromatography regulation, except as otherwise herein provided, the degree of separation between component to be measured and adjacent coexisting substances should be greater than 1.5 according to 2011 editions.Therefore, have only back two kinds of situation can reach the standard-required of degree of separation.
According to said method; With the volume content is organic solvent 15%-30%, and the arbitrary proportion of 0.1% phosphate aqueous solution 70%-85% is formed moving phase, carries out high performance liquid chromatography; Test sample Quzhazhigan peak becomes swarming all can effectively separate with other, and reaches the degree of separation requirement.
4, other testing conditions
According to universal experience, flow rate of mobile phase is selected 1ml/min for use; Chromatogram column temperature is selected 30 ℃ for use; Sampling volume 10 μ l.
Under the above-mentioned condition of determining, about 18 minutes of Quzhazhigan absorption peak retention time; Respectively become swarming can in 60 minutes, all flow out chromatographic column in the Lhasa rhubarb sample chromatogram.Quzhazhigan standard specimen absorption peak theoretical cam curve is greater than 15000, maximum detectability 10ng.Quzhazhigan absorption peak theoretical cam curve is greater than 10000 in the Lhasa rhubarb medicinal material sample determination collection of illustrative plates, and the peak degree of separation meets the requirement of HPLC assay method greater than 1.5.The HPLC collection of illustrative plates of Quzhazhigan sample is seen Fig. 2.
Embodiment 2: the methodology checking of selected condition
1, sample introduction precision
It is an amount of to get the Quzhazhigan reference substance, presses embodiment 1 selected method condition and measures, and wherein moving phase is acetonitrile-0.1% phosphoric acid solution (15: 85), is detected for continuous six times by same analyst, and the record chromatogram is with calculated by peak area RSD.The result sees table 2.
Table 2 sample introduction Precision test result
The result shows that Quzhazhigan peak area and retention time relative standard deviation all are lower than 2%, and instrument accurately and reliably.
According to said method, be organic solvent 15%-30% with the volume content, the arbitrary proportion of 0.1% phosphate aqueous solution 70%-85% is formed moving phase, carries out high performance liquid chromatography, all can reach similar result.
2, repeatability
Get the Lhasa rhubarb test sample, take by weighing six parts by same analyst's precision, press embodiment 1 selected method condition and measure, wherein moving phase is acetonitrile-0.1% phosphoric acid solution (15: 85), and the record chromatogram is asked each part test sample content and relative standard deviation.The result sees table 3.
The repeated result of table 3
The result shows that Quzhazhigan content relative standard deviation is lower than 2%, and method accurately and reliably.
According to said method, be organic solvent 15%-30% with the volume content, the arbitrary proportion of 0.1% phosphate aqueous solution 70%-85% is formed moving phase, carries out high performance liquid chromatography, all can reach similar result.
3, stability of solution
Get the Lhasa rhubarb test sample and the Quzhazhigan reference substance is an amount of; Process need testing solution and reference substance solution in accordance with the law; Measured by embodiment 1 selected method condition at 0,3,6,9,12,24,34 hour respectively, wherein moving phase is acetonitrile-0.1% phosphoric acid solution (15: 85), the record chromatogram; Investigate the stability of reference substance and need testing solution, the result sees table 4.
Table 4 stability test result
The result shows, measures at 34 hours internal reference article solution and need testing solution continuous sample introduction, and its peak area relative standard deviation is illustrated in 34 hours all less than 2% at least, and reference substance solution and need testing solution are stable.
According to said method, be organic solvent 15%-30% with the volume content, the arbitrary proportion of 0.1% phosphate aqueous solution 70%-85% is formed moving phase, carries out high performance liquid chromatography, all can reach similar result.
4, linearity
Precision takes by weighing the about 0.0238g of Quzhazhigan reference substance, puts in the 100ml measuring bottle, adds 75% dissolve with methanol, and is diluted to scale as storing solution.Precision is measured storing solution 0.5ml, 1ml, 2ml, 2.5ml, 3ml, 4ml, 5ml and is put respectively in the 10m measuring bottle; Add the dilution of 75% methyl alcohol and process the solution of a series of gradient concentrations; Measure according to embodiment 1 selected method condition; Wherein moving phase is acetonitrile-0.1% phosphoric acid solution (15: 85), and the result sees table 5.
Table 5 linearity test test findings
Concentration (μ g/ml) with Quzhazhigan is horizontal ordinate, is ordinate with the mean value of peak area, carries out linear regression and calculates, and obtains linear equation: Y=41.74X-47.74 r=0.9999 (n=7)
The result shows that Quzhazhigan sample introduction in concentration is 11.9 μ g/ml-119 μ g/ml concentration ranges presents the good linear relation.
According to said method, be organic solvent 15%-30% with the volume content, the arbitrary proportion of 0.1% phosphate aqueous solution 70%-85% is formed moving phase, carries out high performance liquid chromatography, all can reach similar result.
5, the recovery
The preparation of contrast storing solution: precision takes by weighing Quzhazhigan reference substance 0.0188mg, places the 250ml measuring bottle, adds 75% dissolve with methanol, and is diluted to scale, as storing solution.
The preparation of test sample: get test sample and grind evenly, precision takes by weighing in right amount, places 12 150ml tool plug triangular flasks respectively; Get 3 parts, precision adds 15ml reference substance storing solution respectively, is 80% need testing solution as concentration; Get 3 parts, precision adds 20ml reference substance storing solution respectively, is 100% need testing solution as concentration; Get 3 parts, the respectively accurate 252ml reference substance storing solution that adds is 120% need testing solution as concentration, and according to press the selected method condition mensuration of embodiment 1, wherein moving phase is acetonitrile-0.1% phosphoric acid solution (15: 85), and calculate recovery rate promptly gets, and the result sees table 6.
Quzhazhigan recovery experimental result (n=2) in table 6 Lhasa rhubarb
The result shows, under this chromatographic condition, adopts the average recovery method; By the pharmacopeia requirement, in 80%, 100%, 120% 3 concentration range, every group of parallel three detection recovery population means of concentration are 100.25%; RSD is 1.39%, meets the pharmacopeia requirement, and the result is more satisfactory.
According to said method, be organic solvent 15%-30% with the volume content, the arbitrary proportion of 0.1% phosphate aqueous solution 70%-85% is formed moving phase, carries out high performance liquid chromatography, all can reach similar result.
Embodiment 3: sample size is measured
Pulverizing is meal after getting the Lhasa rhubarb medicinal material drying, and precision takes by weighing 0.1g, puts in the 150ml tool plug triangular flask; Accurately add 75% methyl alcohol 50ml, weigh ultrasonic 30 minutes; Supply the weight that subtracts mistake with 75% methyl alcohol,, be need testing solution with 0.45 μ m membrane filtration.
Chromatographic condition: select the Cosmosil C-18 of Nacalai Tesque company post for use; With acetonitrile-0.1% phosphoric acid solution (15: 85) and methyl alcohol-0.1% phosphoric acid solution (30: 70) is that moving phase is carried out gradient elution, flow velocity 1ml/min; 30 ℃ of column temperatures; Detect wavelength 319nm; Sampling volume 10 μ l.Measure result such as table 7.
The Lhasa rhubarb study sample of table 7 different batches and mensuration result
Through interpretation, in high performance liquid chromatography parameter area of the present invention, the content of Quzhazhigan is same or similar in same batch of study sample.
According to said method, be organic solvent 15%-30% with the volume content, the arbitrary proportion of 0.1% phosphate aqueous solution 70%-85% is formed moving phase, carries out high performance liquid chromatography, all can reach similar result.
Embodiment 4: the experiment of method durability
Get 3 batches of Lhasa rhubarb samples according to embodiment 3 preparation need testing solutions.The condition of measuring: the change flow velocity is 0.95ml/min, and all the other conditions are with embodiment 1, and wherein moving phase is acetonitrile-0.1% phosphoric acid solution (15: 85), measures result such as table 8.Select the condition of another mensuration: changing the detection wavelength is 318nm, and all the other conditions are with embodiment 1, and wherein moving phase is acetonitrile-0.1% phosphoric acid solution (15: 85), measures result such as table 9.
The Lhasa rhubarb study sample of table 8 different batches and mensuration result
The Lhasa rhubarb study sample of table 9 different batches and mensuration result
Experimental result shows, under the constant situation of other conditions, the fine setting flow rate of mobile phase with detect wavelength the result do not had influence.
According to said method, be organic solvent 15%-30% with the volume content, the arbitrary proportion of 0.1% phosphate aqueous solution 70%-85% is formed moving phase, carries out high performance liquid chromatography, all can reach similar result.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (9)
1. efficient liquid-phase chromatography method of measuring Quzhazhigan content in the Lhasa rhubarb; It is characterized in that; The mixed solution of forming with organic solvent and 0.1% phosphate aqueous solution is a moving phase, and it forms volume content is organic solvent 15%-30%, 0.1% phosphate aqueous solution 70%-85%; Carry out high performance liquid chromatography, the content of Quzhazhigan in the analytic sample.
2. efficient liquid-phase chromatography method according to claim 1 is characterized in that, said organic solvent is the mixed solvent of one or more compositions in acetonitrile, methyl alcohol, ether, normal hexane or the cyclohexane.
3. efficient liquid-phase chromatography method according to claim 1 is characterized in that, said organic solvent is an acetonitrile, and forming volume content is acetonitrile 15%, 0.1% phosphate aqueous solution 85%; The type of elution of said high performance liquid chromatography is a gradient elution.
4. efficient liquid-phase chromatography method according to claim 1 is characterized in that, said organic solvent is a methyl alcohol, and forming volume content is methyl alcohol 30%, 0.1% phosphate aqueous solution 70%; The type of elution of said high performance liquid chromatography is a gradient elution.
5. efficient liquid-phase chromatography method according to claim 1 is characterized in that, the chromatographic column filling agent of said high performance liquid chromatography is the carbon octadecyl silane.
6. efficient liquid-phase chromatography method according to claim 1 is characterized in that, the detection wavelength of said high performance liquid chromatography is 319nm.
7. efficient liquid-phase chromatography method according to claim 1 is characterized in that, the chromatographic column column temperature of said high performance liquid chromatography is 30 ℃.
8. efficient liquid-phase chromatography method according to claim 1 is characterized in that, the flow rate of mobile phase of said high performance liquid chromatography is 1.0ml/min.
9. efficient liquid-phase chromatography method according to claim 1 is characterized in that, the sampling volume of said high performance liquid chromatography is 10ul.
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| CN105067562A (en) * | 2015-09-15 | 2015-11-18 | 昆药集团股份有限公司 | Quantitative method of 3,5,3',4'-trihydroxy-stilbene-3'-b-D-glucoside in 3,5,3',4'-trihydroxy-stilbene-3'-b-D-glucoside medicine for injection |
| CN106589007A (en) * | 2016-12-12 | 2017-04-26 | 昆药集团股份有限公司 | Preparation method and test method of CIS for Zhazhi glycoside |
| CN106589007B (en) * | 2016-12-12 | 2019-04-02 | 昆药集团股份有限公司 | Cis- Quzhazhigan and preparation method thereof and detection method |
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