CN106053658B - A kind of Rhizoma drynariae preparata granule characteristic spectrum and its method for building up - Google Patents
A kind of Rhizoma drynariae preparata granule characteristic spectrum and its method for building up Download PDFInfo
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Abstract
The present invention relates to Pharmaceutical Analysis technical field, specially a kind of Rhizoma drynariae preparata granule characteristic spectrum and its method for building up.This feature collection of illustrative plates is using octadecylsilane chemically bonded silica as filler；Using methanol as mobile phase A, using 0.1 v/v% phosphoric acid solutions as Mobile phase B, the regulation according to the form below carries out gradient elution；Detection wavelength is 290nm；Column temperature is 20 DEG C；Flow velocity is 1.0ml per minute.Number of theoretical plate is calculated by aurantiin peak should be not less than 50000.6 characteristic peaks should be presented in test sample characteristic spectrum, relative retention time should be within ± the 5% of specified value.Specified value is：0.299（Peak 1）、0.446（Peak 2）、0.557（Peak 3）、0.579（Peak 4）、0.911（Peak 5）、1.00（Peak 6）.The characteristics of this method is according to granule is reinforced specificity and is differentiated and multicomponent, global quality control, the special characteristic spectrum for establishing the kind, progress overall quality control.
Description
Technical field
The present invention relates to Pharmaceutical Analysis technical field, specially a kind of Rhizoma drynariae preparata granule characteristic spectrum and its foundation
Method.
Background technology
The rhizome of davallia, is the dry rhizome of Plants of Polypodiaceae Mongolian oak fern, analgesic of curing the wound, The strong bone of kidney tonifying, and external application disappears wind nti-freckle, this
The quality standard of medicinal material and its medicine materical crude slice record in《Chinese Pharmacopoeia》Version one in 2015.However, about Rhizoma drynariae preparata granule
But lack corresponding quality standard.
Currently, the open assay method about Rhizoma drynariae preparata granule has《The extraction work of Rhizoma drynariae preparata granule
Skill preferably and its assay》, HPLC is used to measure naringin content, mobile phase methanol-acetic acid-water (35: 4: 65), detection
Wavelength 283nm.As a result:Optimum extraction process is to impregnate 0.5h, adds 10,8 times of amount water to extract 2 times, each 0.5h；Aurantiin quality
Score 0.77%, paste-forming rate 12.6%.Aurantiin is in good linear relationship, mean sample in 0.063-1.575 μ g and peak area
The rate of recovery 100.70%, RSD 1.2%；Tentative this product granule contains aurantiin >=5.0mg per 1g.Conclusion:The extraction process
Stablize feasible, active ingredient extraction efficiency height, for the production and quality control of Rhizoma drynariae preparata granule with content assaying method
Reference is provided.But the document is the extraction process and assay of Rhizoma drynariae preparata granule, assay part is only
The content for measuring aurantiin, does not control other compositions, only carries out assay to some ingredient therein, specially
Attribute is not strong.
Invention content
The present invention is exactly directed to the above technical problem, provides a kind of Rhizoma drynariae preparata granule characteristic spectrum and its foundation side
The characteristics of method, this method is according to granule, reinforces specificity discriminating and multicomponent, global quality control, establishes the kind
Characteristic spectrum, carry out overall quality control.
The specific technical solution of the present invention is as follows：
A kind of method for building up of Rhizoma drynariae preparata granule characteristic spectrum, includes the following steps：
The preparation of reference solution takes 5 hydroxymethyl furfural, protocatechuic acid, aurantiin reference substance appropriate, and methanol is added to be made often
1ml contains the solution of 20 μ g, 80 μ g, 60 μ g to get reference solution respectively；
The preparation of test solution takes Rhizoma drynariae preparata granule appropriate, finely ground, takes 0.2g, accurately weighed, sets tool plug cone
In shape bottle, methanol 50ml is added, close plug, weighed weight is heated to reflux 40 minutes, lets cool, then weighed weight, is supplied and is subtracted with methanol
The weight of mistake, shakes up, and filtration takes filtrate to get test solution；
Accurate absorption reference solution and each 10 μ l of test solution respectively are measured, liquid chromatograph is injected, according to efficient
Liquid chromatography for measuring, record chromatogram is to get Rhizoma drynariae preparata granule characteristic spectrum；
Wherein chromatographic condition is：Using octadecylsilane chemically bonded silica as filler；Using methanol as mobile phase A, with 0.1v/
V% phosphoric acid solutions are Mobile phase B, and gradient elution, Detection wavelength 290nm is carried out in accordance with regulations；Column temperature is 20 DEG C；Flow velocity is every point
Clock 1.0ml.
The condition that gradient elution is carried out in accordance with regulations is：
The percent by volume of 0-10min, mobile phase A are 2%-15%, and the percent by volume of Mobile phase B is 98%-89%；
The percent by volume of 10-15min, mobile phase A are 15%, and the percent by volume of Mobile phase B is 85%；15-27min, mobile phase A
Percent by volume be 15%-27%, the percent by volume of Mobile phase B is 85%-73%；27-35min, the volume of mobile phase A
Percentage is 27%-40%, and the percent by volume of Mobile phase B is 73%-60%；35-50min, the percent by volume of mobile phase A
Percent by volume for 40%-50%, Mobile phase B is 60%-50%.
6 characteristic peaks are presented in this feature collection of illustrative plates for Rhizoma drynariae preparata granule characteristic spectrum, wherein 3 peaks should respectively with
Corresponding object of reference peak retention time is identical, and peak corresponding with aurantiin object of reference peak is the peaks S, calculates the phase of characteristic peak and peak 6
To retention time, relative retention time should be within ± the 5% of specified value.Specified value is：Peak 1,0.299, peak 2,0.446,
Peak 3,0.557, peak 4,0.579, peak 5,0.911, peak 6,1.00.
The positive effect of the present invention is embodied in：
(1), according to granule the characteristics of reinforces specificity discriminating and multicomponent, global quality control, establishes this
The characteristic spectrum of kind carries out overall quality control,
(2), Rhizoma drynariae preparata granule is the extension form of the prepared slices of Chinese crude drugs, loses character specific to medicine materical crude slice and shows
Micro- characteristic, the present invention provide the discriminating of Rhizoma drynariae preparata granule overall chemical ingredient, and specificity is strong.
Description of the drawings
Fig. 1 is the compare feature collection of illustrative plates in embodiment；Wherein, peak 1 is 5 hydroxymethyl furfural, and peak 2 is protocatechuic acid, peak
6 (S) are aurantiin.
Fig. 2 is the selection characteristic spectrum of 1 medium wavelength of embodiment.
Fig. 3 is the selection characteristic spectrum of column temperature in embodiment 1.
Fig. 4 is that Rhizoma drynariae preparata granule mobile phase investigates characteristic spectrum.
Fig. 5 is that Rhizoma drynariae preparata granule chromatographic peak points out characteristic spectrum.
Fig. 6 is the investigation characteristic spectrum of Rhizoma drynariae preparata granule chromatographic column.
Fig. 7 is 7 batches of Rhizoma drynariae preparata granule characteristic spectrums in embodiment.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, right With reference to embodiment
The present invention is described in further detail, but the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to following implementations
Example.
According to high performance liquid chromatography (《Chinese Pharmacopoeia》The one annex VI D of version in 2015) it measures, wherein peak 6 is peak S.
The method for building up of Rhizoma drynariae preparata granule characteristic spectrum：
The preparation of reference solution takes 5 hydroxymethyl furfural, protocatechuic acid, aurantiin reference substance appropriate, and methanol is added to be made often
1ml contains the solution of 20 μ g, 80 μ g, 60 μ g to get reference solution respectively.
The preparation of test solution takes this product appropriate, finely ground, takes about 0.2g, accurately weighed, sets in conical flask with cover, accurate
Methanol 50ml is added, close plug, weighed weight is heated to reflux 40 minutes, lets cool, then weighed weight, and the weight of less loss is supplied with methanol
Amount, shakes up, and filters, takes subsequent filtrate to get test solution.
Measuring method is accurate respectively to draw reference solution and each 10 μ l of test solution, injects liquid chromatograph, measures, note
Chromatogram is recorded to get Rhizoma drynariae preparata granule characteristic spectrum；
Wherein chromatographic condition is：With octadecylsilane chemically bonded silica (Féraud door Luna C18 (2) 100A4.6 ×
250mm, 5 μm) it is filler；Using methanol as mobile phase A, using 0.1v/v% phosphoric acid solutions as Mobile phase B, gradient is carried out in accordance with regulations
Elution, Detection wavelength 290nm；Column temperature is 20 DEG C；Flow velocity is 1.0ml per minute, and number of theoretical plate should not by the calculating of aurantiin peak
Less than 50000.
The condition that gradient elution is wherein carried out in accordance with regulations is：
The percent by volume of 0-10min, mobile phase A are 2%-15%, and the percent by volume of Mobile phase B is 98%-89%；
The percent by volume of 10-15min, mobile phase A are 15%, and the percent by volume of Mobile phase B is 85%；15-27min, mobile phase A
Percent by volume be 15%-27%, the percent by volume of Mobile phase B is 85%-73%；27-35min, the volume of mobile phase A
Percentage is 27%-40%, and the percent by volume of Mobile phase B is 73%-60%；35-50min, the percent by volume of mobile phase A
Percent by volume for 40%-50%, Mobile phase B is 60%-50%.
6 characteristic peaks should be presented in test sample characteristic spectrum, wherein when 3 peaks should retain with corresponding object of reference peak respectively
Between it is identical, peak corresponding with aurantiin object of reference peak is the peaks S, calculates the relative retention time of characteristic peak and the peaks S, opposite reservation
Time should be within ± the 5% of specified value.Specified value is：0.299 (peak 1), 0.446 (peak 2), 0.557 (peak 3), 0.579 (peak
4), 0.911 (peak 5), 1.00 (peak 6 is also peak S), specific compare feature collection of illustrative plates is shown in Fig. 1, the liquid of the Rhizoma drynariae preparata granule
The foundation of phase character collection of illustrative plates can be used as the global quality control method of Rhizoma drynariae preparata granule.
Embodiment 1：
1, material, reagent and instrument
1.1 laboratory apparatus
Agilent 1200series high performance liquid chromatographs；
Chromatographic column：Féraud door luna 5u C18 (2) 4.6*250mm (methodological study)
1.2 reagents and reagent
Methanol is chromatographically pure, and water is ultra-pure water, remaining reagent is that analysis is pure.
Aurantiin (Nat'l Pharmaceutical ＆ Biological Products Control Institute 110722-201312, content 94.7%), 5 hydroxymethyl furfural
(Nat'l Pharmaceutical ＆ Biological Products Control Institute 111626-201509, content 97.8%), protocatechuic acid (middle inspection institute 110809-
200604),
Rhizoma drynariae preparata granule (lot number：New green 1501087,1403058,1408098,1404042,1509078,
1404172、1409058)
2, the preparation of test solution
The Rhizoma drynariae preparata granule of the above lot number is prepared into confession according to the preparation method of test solution in embodiment
The test solution of the present embodiment detection.
3, chromatographic condition and system suitability
Using octadecylsilane chemically bonded silica as filler (Féraud door Luna C18 (2) 4.6 × 250mm of 100A, 5 μm)；
Using methanol as mobile phase A, using 0.1v/v% phosphoric acid solutions as Mobile phase B, the regulation according to the form below carries out gradient elution；Detect wave
A length of 290nm；Column temperature is 20 DEG C；Flow velocity is 1.0ml per minute.Number of theoretical plate is calculated by aurantiin peak should be not less than 50000.Stream
Dynamic property gradient elution table is shown in Table 1.
1 mobility gradient elution table of table
3.1 wavelength selection：It compares under Detection wavelength 283nm, 263nm, 254nm, 290nm, 300nm, 330nm, 220nm
Chromatographic peak, and the separating degree between chromatographic peak score at 290nm is more and each peak is preferable, contains much information, and baseline is steady,
Therefore Detection wavelength is determined as 290nm, sees Fig. 2.
3.2 column temperatures are investigated：20 DEG C are compared, 25 DEG C, as a result 30 DEG C of chromatogram shows 20 DEG C of chromatographic peak peak shape the most
Symmetrically, separating degree is best, therefore column temperature is determined as 20 DEG C, sees Fig. 3.
3.3 mobile phases select：The separating effect of 3 kinds of different mobile phases has been investigated in this experiment, respectively：I：Methanol-water-vinegar
Sour gradient elution (official method)；II：Acetonitrile -0.1%v/v phosphoric acid gradient elutions；Ⅲ：Methanol -0.1v/v% phosphoric acid gradients are washed
It is de-.The result shows that：
Chromatographic peak is more under mobile phase III separation conditions, and number of theoretical plate, separating degree, symmetry are more preferable, therefore by mobile phase
Mobile phases of the III as Rhizoma drynariae preparata granule characteristic spectrum assay method.As a result such as Fig. 4.
4, chromatographic peak is pointed out
It is positioned using reference substances such as aurantiin, 5 hydroxymethyl furfural, protocatechuic acid, the results showed that：Peak 1 is 5- hydroxyl first
Base furfural, peak 2 are protocatechuic acid, and peak 6 is aurantiin.See Fig. 5.
5, methodological study
5.1 sample introduction precision tests
Take Rhizoma drynariae preparata granule (lot number：1501087) test solution, continuous sample introduction 6 times, 10 μ l every time, with peak 1
(5 hydroxymethyl furfural), peak 2 (protocatechuic acid), peak 3, peak 4, peak 5 are calculated as index peak with the opposite of peak 6 (S) (aurantiin)
Retention time and relative peak area, as a result the RSD of relative retention time and relative peak area be respectively less than 2.0%, show this method
Sample introduction precision is good.It is shown in Table 2 and table 3.
2 sample introduction precision investigation of table-characteristic peak relative retention time ratio
3 sample introduction precision investigation of table-characteristic peak relative peak area ratio
5.2 repeatability are investigated
Precision weighs 6 parts of Rhizoma drynariae preparata granule (lot number 1501087), is prepared and is surveyed according to the method for drafting
Fixed, as a result the relative retention time at each index feature peak and the RSD of relative peak area are respectively less than 2.0%, show that this method repeats
Property is good.It is shown in Table 4 and table 5.
Repeated investigation-characteristic peak relative retention time the ratio of table 4
Repeated investigation-characteristic peak relative peak area the ratio of table 5
5.3 stabilities of solution are investigated
Same test solution is taken, respectively at 0,2,5,8,15, it measures for 24 hours, characteristic peak therein is analyzed,
Corresponding chromatographic peak relative retention time is respectively less than 2.0%, and the RSD of the relative peak area of characteristic peak is respectively less than 2.0%, as a result
Show that test solution is stablized interior for 24 hours.It is shown in Table 6 and table 7.
6 study on the stability of table-characteristic peak relative retention time
7 study on the stability of table-characteristic peak relative peak area ratio
5.4 durabilities are investigated
5.4.1 chromatographic column durability using different brands and length C18 chromatographic columns according to the method drafted to this product into
Row characteristic spectrum detects, and as a result the relative retention time at Partial Feature peak exceeds prescribed limit, the results showed that this method is to difference
The durability of brand and length chromatographic column is poor, therefore stationary chromatographic column is answered to be measured.Féraud is fixed in ultimate criterion text
This brand chromatographic column of door luna 5u C18 (2) 4.6*250mm is detected, and sees Fig. 6.
6, the determination of characteristic peak and the foundation of control collection of illustrative plates
The measurement that using the method drafted the 7 batches of samples of this product are carried out with characteristic spectrum, according to relative retention time it is stable and
The principle that each enterprise's each batch sample can detect and peak is relatively high, has selected 5 preferable peaks of repeatability as feature altogether
Peak.Final regulation：5 characteristic peaks should be presented in test sample characteristic spectrum, wherein 2 peaks should be protected with corresponding object of reference peak respectively
Stay the time identical, peak corresponding with aurantiin object of reference peak is the peaks S, calculates the relative retention time of characteristic peak and the peaks S, opposite
Retention time should be within ± the 5% of specified value.Specified value is：0.446 (peak 1), 0.557 (peak 2), 0.579 (peak 3), 0.911
(peak 4), 1.00 (peaks 6).It is shown in Table 8.
87 batches of Rhizoma drynariae preparata granule relative retention times of table
7 batches of samples are synthesized using similarity evaluation (2012 editions), are established boiling hot
The control collection of illustrative plates of rhizome of davallia granule characteristic spectrum, is shown in Fig. 7.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
Claims (1)
1. a kind of method for building up of Rhizoma drynariae preparata granule characteristic spectrum, it is characterised in that include the following steps：
The preparation of reference solution takes 5 hydroxymethyl furfural, protocatechuic acid, aurantiin reference substance appropriate, adds methanol that every 1ml is made
Contain the solution of 20 μ g, 80 μ g, 60 μ g respectively to get reference solution；
The preparation of test solution takes Rhizoma drynariae preparata granule appropriate, finely ground, takes 0.2g, accurately weighed, sets conical flask with cover
In, methanol 50ml is added, close plug, weighed weight is heated to reflux 40 minutes, lets cool, then weighed weight, and less loss is supplied with methanol
Weight shakes up, and filtration takes filtrate to get test solution；
Accurate absorption reference solution and each 10 μ l of test solution respectively are measured, liquid chromatograph is injected, according to efficient liquid phase
Chromatography determination, record chromatogram is to get Rhizoma drynariae preparata granule characteristic spectrum；
Wherein chromatographic condition is：Chromatographic column is 2 100A 4.6 × 250mm of Féraud door Luna C18,5 μm；It is flowing with methanol
Gradient elution, Detection wavelength 290nm is carried out in accordance with regulations using 0.1 v/v% phosphoric acid solutions as Mobile phase B in phase A；Column temperature is 20
℃；Flow velocity is 1.0ml per minute；6 characteristic peaks are presented in characteristic spectrum, wherein 3 peaks should respectively with corresponding object of reference peak
Retention time is identical, and peak corresponding with aurantiin object of reference peak is the peaks S, calculates the relative retention time of characteristic peak and peak 6, phase
It is to retention time：Peak 1,0.299, peak 2,0.446, peak 3,0.557, peak 4,0.579, peak 5,0.911, peak 6,1.00；It is described
The condition of gradient elution is：
The percent by volume of 0-10min, mobile phase A are 2%-15%, and the percent by volume of Mobile phase B is 98%-85%；
The percent by volume of 10-15min, mobile phase A are 15%, and the percent by volume of Mobile phase B is 85%；
The percent by volume of 15-27min, mobile phase A are 15%-27%, and the percent by volume of Mobile phase B is 85%-73%；
The percent by volume of 27-35min, mobile phase A are 27%-40%, and the percent by volume of Mobile phase B is 73%-60%；
The percent by volume of 35-50min, mobile phase A are 40%-50%, and the percent by volume of Mobile phase B is 60%-50%.
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| CN109799306B (en) * | 2019-03-29 | 2021-06-22 | 四川新绿色药业科技发展有限公司 | High performance liquid chromatography method for detecting characteristic spectrums of fried cowherb seed decoction pieces, standard decoction and formula granules |
| CN112946111B (en) * | 2021-01-29 | 2023-01-17 | 广东一方制药有限公司 | Method for constructing and identifying UPLC fingerprint of rhizoma Drynariae crude product and its processed product |
| CN116270770B (en) * | 2023-03-01 | 2024-07-26 | 岭南中药饮片有限公司 | Preparation method of drynaria rhizome formula particles |
| CN117607312A (en) * | 2024-01-19 | 2024-02-27 | 北京岐黄制药有限公司 | Construction method and application of drynaria total flavone feature map |
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