CN102507830B - 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 analytical chemistry field, particularly a kind of efficient liquid-phase chromatography method of measuring Quzhazhigan content in Lhasa rhubarb.
Background technology
Lhasa rhubarb Rheum lhasaense A.J.Li et P.K.Hsiao is Rheum ripple leaf group plant.Tibetan is among the people with herbal medicine, hides and is named as bent letter, dries and is used as medicine with rhizome.In " newly repairing Jingzhubencao ", classified as " sub-rheum officinale ", commonly use kind for one of " bent letter " medicinal material, its root and rhizome is used as medicine.In " Bao Shu complies with one's wishes ", say " sub-rheum officinale is slow, sharp, and voltinism is flat ".Wild Lhasa rhubarb main product is in China Tibet, Sichuan and other places.By early-stage Study, we have found the active component Quzhazhigan in Lhasa rhubarb, have the effect for the treatment of 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-(3,5-dihydroxyphenyl)-2-(3-hydroxyl-4-O-β-D-glucopyranose phenyl) ethene, or become 3,5,3 ', 4 '-tetrahydroxy Stilbene-3 '-O-beta-glucosidase (having again 3,5, the 4 '-trihydroxy-Stilbene-3 '-O-glucoside of title).Chemical structural drawing is as follows:
Conventional detection with separate Lhasa rhubarb in the method for Quzhazhigan comprise high performance liquid chromatography etc.High performance liquid chromatography (High Performance Liquid Chromatography HPLC) claims again " high pressure liquid chromatography ", " high-speed liquid chromatography ", " high separation liquid chromatography ", " column chromatography in modern age " etc.High performance liquid chromatography is a chromatographic important branch, take liquid as mobile phase, adopt high pressure transfusion system, pump into by thering is the single solvent of opposed polarity or the mobile phase such as mixed solvent, damping fluid of different proportion the chromatographic column that fixing phase is housed, in post each composition separated after, enter detecting device and detect, thereby realize the analysis to sample.
But at present, in utilizing high performance liquid chromatography detection and separating Lhasa rhubarb, in the method for Quzhazhigan, exist some problems and shortcoming.Such as, cannot with other compositions effective separate, do not reach degree of separation require etc.By research, these are all relevant with composition and the ratio of selected mobile phase.Therefore, find a kind of suitable use high performance liquid chromatography to detect and 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 problem to be solved in the present invention is the low problem of degree of separation existing for the HPLC analytical method of Quzhazhigan in prior art, and the method for Quzhazhigan content in a kind of Accurate Determining 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 Lhasa rhubarb, take the mixed solution of organic solvent and 0.1% phosphate aqueous solution composition as mobile phase, its composition 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 analytic sample.
High-performance liquid chromatogram determination of the present invention selects the most frequently used carbon octadecyl silane post to carry out stratographic analysis.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., all has better separating effect.
In one embodiment of the invention, inventor measures ultraviolet spectrum by getting after Quzhazhigan reference substance methyl alcohol dissolves, and determines the detection wavelength of high performance liquid chromatography.Experimental result shows, large but approach end absorption region in the absorption value of 200nm and 216nm, absorption value maximum and the absorption peak at 318.5nm place are more smooth, therefore detection wavelength is selected 319nm.
According to conventional method, the flow rate of mobile phase of efficient liquid-phase chromatography method of the present invention is selected 1ml/min; Chromatogram column temperature is selected 30 ℃; Sampling volume is selected 10ul.
In one embodiment of the invention, inventor has compared different mobile phases, and the mobile phase of different proportion is on detecting the impact of separating effect.Experimental result shows, in the situation that other conditional parameters are constant, mixes the mobile phase of composition with first alcohol and water according to the ratio of 40: 60, and in test sample, Quzhazhigan becomes swarming to separate bad with other; Mix the mobile phase of composition according to the ratio of 20: 80 with acetonitrile and water, in test sample, Quzhazhigan becomes swarming to separate bad with other; The mobile phase that mixes composition according to the ratio of 10: 90 with acetonitrile and 0.1% phosphoric acid solution carries out gradient elution, though Quzhazhigan and other compositions and other component separating in 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: the mobile phase that between 70-85, arbitrary proportion mixes composition carries out gradient elution, in test sample, Quzhazhigan can effectively separate with other compositions, and reaches 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, in the present invention, organic solvent is the solvent mixture of one or more compositions in acetonitrile, methyl alcohol, ether, normal hexane or cyclohexane.
More preferably, in the present invention, organic solvent is acetonitrile or methyl alcohol.
In an embodiment of the present invention, inventor has carried out methodology checking to above-mentioned selected parameter.Comprising the precision of checking sample introduction, the repeatability of method, the stability of solution, linearity and the recovery of method.Experimental result shows, the selected high performance liquid chromatography parameter of the present invention can meet the detection separation requirement to Quzhazhigan in sample.
In an embodiment of the present invention, 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, in same batch of study sample, the content of Quzhazhigan is same or similar.
Major advantage of the present invention is as follows:
(1) the present invention, through systematic comparison research, has set up the efficient liquid-phase chromatography method of measuring Quzhazhigan content in Lhasa rhubarb first;
(2) technical characterstics such as the method in the present invention has good separating effect, measures accurately, highly sensitive, and specificity is strong, analytical approach is easy;
(3) variation that the method in the present invention is planted, stored, extracts effective constituent Quzhazhigan in the processes such as processing accurate grasp kind, has direct using value.
Accompanying drawing explanation
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 Lhasa rhubarb, those skilled in the art can use for reference content herein, suitably improve technological parameter and realize.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the artly, they are all deemed to be included in the present invention.Method of the present invention and application are described by preferred embodiment, related personnel obviously can change methods and applications as herein described in content of the present invention, spirit and scope or suitably change and combination not departing from, and realizes and apply the 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, be organic solvent 15%-30% by volume content, the mixed solution of the organic solvent-0.1% phosphate aqueous solution composition of 0.1% phosphate aqueous solution 70%-85% is that mobile phase carries the compositions such as Quzhazhigan and enters chromatographic column, chromatographic column take carbon octadecyl silane as filling agent separates Quzhazhigan with other chemical compositions, make it arrive successively UV-detector detected identification; Detecting device is measured the response at Quzhazhigan peak in Lhasa rhubarb sample, and respectively corresponding its sample size is how many, by the size of its response and the content that relatively calculates Quzhazhigan in Lhasa rhubarb sample of Quzhazhigan standard specimen.
In order to make those skilled in the art understand better technical scheme of the present invention, below in conjunction with specific embodiment, the present invention is described in further detail.
The instrument that following examples adopt and tested medicine:
Instrument: Shimadzu 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; 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, selecting of chromatographic column
Consider the ubiquity of application, select HPLC to measure the most frequently used carbon octadecyl silane post.Compare 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., all had better separating effect.
2, detecting wavelength determines
Get after Quzhazhigan reference substance methyl alcohol dissolves and measure ultraviolet spectrum, the results are shown in Figure 1, there is ultraviolet absorption curve, have three main absorption bands.Wherein the absorption value of 200nm and 216nm is large but approach end absorption region, and absorption value maximum and the absorption peak at 318.5nm place are more smooth, therefore detection wavelength is selected 319nm.
3, the selection of mobile phase
Lhasa rhubarb complicated component, selects suitable mobile phase to obtain the key that good separating effect is analytical approach.Select the flow phase system such as methanol-water, acetonitrile-water to contrast screening, all cannot separate the Related Component in Lhasa rhubarb completely.According to the variation tendency at major component peak, mobile phase is adjusted into organic solvent-0.1% phosphate aqueous solution, be organic solvent 15%-30% according to volume content, the mobile phase of the ratio composition of 0.1% phosphate aqueous solution 70%-85% carries out gradient elution, have good separating effect, test findings is in table 1.
Table 1 mobile phase contrast shaker test data
According to 2011 editions " Chinese Pharmacopoeias " appendix VI 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.Therefore, only have latter two situation can reach the standard-required of degree of separation.
According to said method, take volume content as organic solvent 15%-30%, the arbitrary proportion composition mobile phase of 0.1% phosphate aqueous solution 70%-85%, carries out high performance liquid chromatography, test sample Quzhazhigan peak becomes swarming all can effectively separate with other, and reaches degree of separation requirement.
4, other testing conditions
According to universal experience, flow rate of mobile phase is selected 1ml/min; Chromatogram column temperature is selected 30 ℃; Sampling volume 10 μ l.
Under the above-mentioned condition of determining, Quzhazhigan absorption peak retention time approximately 18 minutes; In Lhasa rhubarb sample chromatogram, each one-tenth swarming can all flow out chromatographic column in 60 minutes.Quzhazhigan standard specimen absorption peak theoretical cam curve is greater than 15000, maximum detectability 10ng.In Lhasa rhubarb medicinal material sample determination collection of illustrative plates, Quzhazhigan absorption peak theoretical cam curve is greater than 10000, and peak degree of separation is greater than 1.5, meets the requirement of HPLC assay method.Fig. 2 is shown in by the HPLC collection of illustrative plates of Quzhazhigan sample.
Embodiment 2: the methodology checking of selected condition
1, sample introduction precision
Get Quzhazhigan reference substance appropriate, measure by the method condition that embodiment 1 is selected, wherein mobile phase is acetonitrile-0.1% phosphoric acid solution (15: 85), is detected for continuous six times by same analyst, records chromatogram, with calculated by peak area RSD.The results are shown in Table 2.
Table 2 sample introduction Precision test result
Result shows that Quzhazhigan peak area and retention time relative standard deviation are all lower than 2%, and instrument accurately and reliably.
According to said method, take volume content as organic solvent 15%-30%, the arbitrary proportion composition mobile phase of 0.1% phosphate aqueous solution 70%-85%, carries out high performance liquid chromatography, all can reach similar result.
2, repeatability
Get Lhasa rhubarb test sample, take six parts by same analyst's precision, measure by the method condition that embodiment 1 is selected, wherein mobile phase is acetonitrile-0.1% phosphoric acid solution (15: 85), record chromatogram, ask each part of test sample content and relative standard deviation.The results are shown in Table 3.
The repeated result of table 3
Result shows that Quzhazhigan content relative standard deviation is lower than 2%, and method accurately and reliably.
According to said method, take volume content as organic solvent 15%-30%, the arbitrary proportion composition mobile phase of 0.1% phosphate aqueous solution 70%-85%, carries out high performance liquid chromatography, all can reach similar result.
3, stability of solution
Get Lhasa rhubarb test sample and Quzhazhigan reference substance is appropriate, make need testing solution and reference substance solution in accordance with the law, measured by the selected method condition of embodiment 1 at 0,3,6,9,12,24,34 hour respectively, wherein mobile phase is acetonitrile-0.1% phosphoric acid solution (15: 85), record chromatogram, the stability of investigating reference substance and need testing solution, the results are shown in Table 4.
Table 4 stability test result
Result shows, measures at 34 hours internal reference product solution and need testing solution continuous sample introduction, and its peak area relative standard deviation is all less than 2%, shows at least 34 hours, and reference substance solution and need testing solution are stable.
According to said method, take volume content as organic solvent 15%-30%, the arbitrary proportion composition mobile phase of 0.1% phosphate aqueous solution 70%-85%, carries out high performance liquid chromatography, all can reach similar result.
4, linearity
Precision takes the about 0.0238g of Quzhazhigan reference substance, puts in 100ml measuring bottle, adds 75% methyl alcohol and dissolves, and be diluted to scale as storing solution.Precision measures storing solution 0.5ml, 1ml, 2ml, 2.5ml, 3ml, 4ml, 5ml and puts respectively in 10m measuring bottle, add 75% methyl alcohol dilution and make the solution of a series of gradient concentrations, measure according to the method condition that embodiment 1 is selected, wherein mobile phase is acetonitrile-0.1% phosphoric acid solution (15: 85), the results are shown in Table 5.
Table 5 linearity test test findings
Take the concentration (μ g/ml) of Quzhazhigan as horizontal ordinate, take the mean value of peak area as ordinate, carry out linear regression calculating, obtain linear equation: Y=41.74X-47.74 r=0.9999 (n=7)
Result shows that Quzhazhigan sample introduction in concentration is 11.9 μ g/ml-119 μ g/ml concentration ranges presents good linear relation.
According to said method, take volume content as organic solvent 15%-30%, the arbitrary proportion composition mobile phase of 0.1% phosphate aqueous solution 70%-85%, carries out high performance liquid chromatography, all can reach similar result.
5, the recovery
The preparation of contrast storing solution: precision takes Quzhazhigan reference substance 0.0188mg, is placed in 250ml measuring bottle, adds 75% methyl alcohol to dissolve, and is diluted to scale, as storing solution.
The preparation of test sample: get test sample and grind evenly, precision takes in right amount, is placed in respectively 12 150ml tool plug triangular flasks; Get 3 parts, precision adds 15ml reference substance storing solution, the need testing solution that is 80% as concentration respectively; Get 3 parts, precision adds 20ml reference substance storing solution, the need testing solution that is 100% as concentration respectively; Get 3 parts, precision adds 252ml reference substance storing solution, the need testing solution that is 120% as concentration respectively, measure according to pressing the selected method condition of embodiment 1, wherein mobile phase is acetonitrile-0.1% phosphoric acid solution (15: 85), and calculate recovery rate and get final product the results are shown in Table 6.
Quzhazhigan recovery experimental result (n=2) in table 6 Lhasa rhubarb
Result shows, under this chromatographic condition, adopts average recovery method, by 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 pharmacopeia requirement, and result is more satisfactory.
According to said method, take volume content as organic solvent 15%-30%, the arbitrary proportion composition mobile phase of 0.1% phosphate aqueous solution 70%-85%, carries out high performance liquid chromatography, all can reach similar result.
Embodiment 3: sample size is measured
After getting Lhasa rhubarb medicinal material drying, pulverize as meal, precision takes 0.1g, puts in 150ml tool plug triangular flask, accurately add 75% methyl alcohol 50ml, weigh, ultrasonic 30 minutes, supply the weight of less loss with 75% methyl alcohol, with 0.45 μ m membrane filtration, be need testing solution.
Chromatographic condition: select the Cosmosil C-18 of Nacalai Tesque company post; Carry out gradient elution, flow velocity 1ml/min take acetonitrile-0.1% phosphoric acid solution (15: 85) and methyl alcohol-0.1% phosphoric acid solution (30: 70) as mobile phase; 30 ℃ of column temperatures; Detect wavelength 319nm; Sampling volume 10 μ l.Measurement result is as table 7.
Lhasa rhubarb study sample and the measurement result of table 7 different batches
Interpretation of result by experiment, in high performance liquid chromatography parameter area of the present invention, in same batch of study sample, the content of Quzhazhigan is same or similar.
According to said method, take volume content as organic solvent 15%-30%, the arbitrary proportion composition mobile phase of 0.1% phosphate aqueous solution 70%-85%, carries out high performance liquid chromatography, all can reach similar result.
Embodiment 4: method durability experiment
Get 3 batches of Lhasa rhubarb samples and prepare need testing solution according to embodiment 3.The condition of measuring: change flow velocity is 0.95ml/min, and all the other conditions are with embodiment 1, and wherein mobile phase is acetonitrile-0.1% phosphoric acid solution (15: 85), and measurement result is as table 8.Select the condition of another mensuration: changing detection wavelength is 318nm, and all the other conditions are with embodiment 1, and wherein mobile phase is acetonitrile-0.1% phosphoric acid solution (15: 85), and measurement result is as table 9.
Lhasa rhubarb study sample and the measurement result of table 8 different batches
Lhasa rhubarb study sample and the measurement result of table 9 different batches
Experimental result shows, in the situation that other conditions are constant, fine setting flow rate of mobile phase and detect wavelength on result without impact.
According to said method, take volume content as organic solvent 15%-30%, the arbitrary proportion composition mobile phase of 0.1% phosphate aqueous solution 70%-85%, carries out high performance liquid chromatography, all can reach similar result.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (3)
1. measure the efficient liquid-phase chromatography method of Quzhazhigan content in Lhasa rhubarb for one kind, it is characterized in that, take the mixed solution of organic solvent and 0.1% phosphate aqueous solution composition as mobile phase, its composition 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 analytic sample, described organic solvent is the mixed solvent of one or both compositions in acetonitrile or methyl alcohol; The chromatographic column filling agent of described high performance liquid chromatography is carbon octadecyl silane;
The detection wavelength of high performance liquid chromatography is 319nm, and chromatographic column column temperature is 30 ℃, and flow rate of mobile phase is 1.0ml/min, and sampling volume is 10 μ l.
2. efficient liquid-phase chromatography method according to claim 1, is characterized in that, described organic solvent is acetonitrile, and composition volume content is acetonitrile 15%, 0.1% phosphate aqueous solution 85%.
3. efficient liquid-phase chromatography method according to claim 1, is characterized in that, described organic solvent is methyl alcohol, and composition volume content is methyl alcohol 30%, 0.1% phosphate aqueous solution 70%.
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| CN103713067B (en) * | 2014-01-08 | 2015-06-17 | 昆药集团股份有限公司 | Ultra-high performance liquid chromatography method for determining content of rheum lhasaense |
| 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 |
| 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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