CN109507310A - Support the fingerprint map construction method and detection method of the beautiful prescription of essence kind - Google Patents
Support the fingerprint map construction method and detection method of the beautiful prescription of essence kind Download PDFInfo
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Abstract
The present invention discloses the fingerprint map construction method and detection method of the beautiful prescription of breeding essence kind.The construction method includes the following steps: prepared by test solution；Reference substance solution preparation；The building of finger-print: drawing the test solution, reference substance solution, and injection high performance liquid chromatograph measurement obtains the beautiful prescription finger-print of feeding essence kind with common characteristic peaks.Inventor is on the basis of permanent experience accumulation and after many experiments, it selects ferulic acid, Paeoniflorin, morroniside, loganin and is used as and construct finger-print referring to product, the quality of Zhong Yu decoction this classical dosage form can not only be characterized well but also the quality that its Modern preparations supports the beautiful soft extracts of essence kind, supports the beautiful granule of essence kind can be characterized.In particular, cooperation selects suitable chromatographic condition to construct finger-print, can not only qualitative, quantitatively characterizing Zhong Yu decoction, and characterization that can also be qualitative, quantitative supports the beautiful soft extracts of essence kind, supports the beautiful granule of essence kind.
Description
Technical field
The present invention relates to Chinese materia medica preparation field of quality control, more particularly to the fingerprint map construction side of the beautiful prescription of feeding essence kind
Method and detection method.
Background technique
Zhong Yu decoction is traditional Chinese medicinal formulae, and on "Fu Qingzhu works on obstetric" volume, prescription is 30 grams of big radix rehmanniae preparata
(nine steam), 15 grams of Radix Angelicae Sinensis (wine is washed), 15 grams of Radix Paeoniae Alba (parched with wine), 15 grams of pulp of dogwood fruit (cooking), are mainly used for kidney asthenia and blood deficiency, body is thin
It is weak, it fails to be impregnated for a long time.
The preparation of feeding smart kind of jade side on sale, which has, currently on the market supports the beautiful soft extracts of essence kind and supports the beautiful particle of essence kind, has document
Finger-print and assay research have been carried out to the beautiful soft extracts of feeding essence kind, assay research has been carried out to the beautiful particle of feeding essence kind,
But research is only the finger-print comparative approach for establishing the more batches of feeding beautiful soft extracts of essence kind respectively, and to the Chinese herbaceous peony in soft extracts and granule
Two ingredients of medicine glycosides and loganin establish assay.The detection of preparation about feeding smart kind of jade side, there is presently no systems
One method standard measures decoction, granule, soft extracts comprehensively.
It would therefore be highly desirable to provide a kind of unified method to Zhong Yu decoction agent, support the beautiful granule of essence kind, support the beautiful soft extracts of essence kind
It is measured etc. the beautiful prescription of feeding essence kind.
Summary of the invention
Based on this, the main object of the present invention is to provide the construction method of the finger-print of the beautiful prescription of breeding essence kind.
The main object of the present invention is achieved through the following technical solutions:
The construction method of the finger-print of the beautiful prescription of one breeding essence kind, the construction method include the following steps:
Test solution preparation: it rests the beautiful decoction of essence kind and is prepared into freeze-dried powder, the freeze-dried powder is dissolved in organic solvent, mistake
Filter, obtains test solution；
Reference substance solution preparation: ferulic acid, Paeoniflorin, morroniside, loganin reference substance are dissolved in organic solvent, must be compareed
Product solution；
The building of finger-print: drawing the test solution, reference substance solution, and injection high performance liquid chromatograph is surveyed
It is fixed, obtain the beautiful prescription finger-print of feeding essence kind with common characteristic peaks.
In wherein some embodiments, the chromatographic condition that the measurement uses includes:
Chromatographic column: using octadecylsilane chemically bonded silica as filler；
Mobile phase: using acetonitrile as mobile phase A, the phosphate aqueous solution for being 0.08%~0.12% using volumetric concentration is mobile phase
B；
Gradient elution mode: the percentage by volume of 0min~25min, mobile phase A are changed to 15% by 5%, Mobile phase B
Percentage by volume is changed to 85% by 95%；Mobile phase is by 25min~40min, and the percentage by volume of mobile phase A is by 15% variation
To 20%, the percentage by volume of Mobile phase B is changed to 80% by 85%；40min~60min, the percentage by volume of mobile phase A by
20% is changed to 50%, and the percentage by volume of Mobile phase B is changed to 50% by 80%.
In wherein some embodiments, the flow velocity of the mobile phase is 0.8mL/min~1.2mL/min；The color
The column temperature for composing column is 25 DEG C~35 DEG C；The Detection wavelength used that measures is 210nm~250nm.
In wherein some embodiments, the organic solvent is the methanol solution that volumetric concentration is 70%~100%.
In wherein some embodiments, be added in organic solvent described in every 25mL~50mL the freeze-dried powder 0.5g~
1g。
In wherein some embodiments, the preparation of the freeze-dried powder includes:
Rehmannia glutinosa, prepared RADIX ANGELICAE SINENSIS with yellow rice wine, stir-baked RADIX PAEONIAE ALBA with vino, wine-prepared fructus corni medicine materical crude slice are taken, mixes, is soaked in water 30 points by weight for 2:1:1:1
Clock；Decoct twice: for the first time plus water is 8 times of medicine materical crude slice total weight, is decocted 1 hour, filtration, filtrate is spare；For the second time plus water is
8 times of medicine materical crude slice total weight decoct 1 hour, filtration, and filtrate decocts gained filtrate with first time and merges, and are concentrated under reduced pressure into inventory
With concentrate weight than the clear cream for 1:1~1:1.5 after, be added account for the clear cream weight be 7%~15% superfine silica gel powder,
Powder is lyophilized into -20 DEG C to -45 DEG C pre-freezes, then under conditions of -80 DEG C, < 100Pa to get freeze-dried powder.
In wherein some embodiments, 0.6 μ g of μ g~24 of ferulic acid, Paeoniflorin 2.1 are contained in contrast solution described in every 1mL
μ g of μ g~84.2,2.0 μ g of μ g~80.6 of morroniside, 2.5 μ of μ g~101.3 g of loganin.
It is a further object of the present invention to provide the measuring method of the beautiful prescription of breeding essence kind, which includes following step
It is rapid:
Test solution preparation: the feeding beautiful prescription of essence kind to be measured is dissolved in organic solvent, filters, obtains test solution；
Reference substance solution preparation: ferulic acid, Paeoniflorin, morroniside, loganin reference substance are dissolved in organic solvent, must be compareed
Product solution；
Test solution measurement: drawing the test solution, reference substance solution, and injection high performance liquid chromatograph carries out
Measurement obtains the map of the beautiful prescription of feeding essence kind to be measured；Compare the map of the feeding beautiful prescription of essence kind to be measured and the finger of Chinese fir building
The peak area at the relative retention time at each peak and/or each peak in line map, complete to the qualitative of the feeding beautiful prescription of essence kind to be measured and/or
Quantitative determination.
The beautiful prescription of feeding essence kind of the present invention includes granule, medicinal extract, decoction.
In wherein some embodiments, the chromatographic condition that the measurement uses includes:
Chromatographic column: using octadecylsilane chemically bonded silica as filler；
Mobile phase: using acetonitrile as mobile phase A, the phosphate aqueous solution for being 0.08%~0.12% using volumetric concentration is mobile phase
B；
Gradient elution mode: the percentage by volume of 0min~25min, mobile phase A are changed to 15% by 5%, Mobile phase B
Percentage by volume is changed to 85% by 95%；Mobile phase is by 25min~40min, and the percentage by volume of mobile phase A is by 15% variation
To 20%, the percentage by volume of Mobile phase B is changed to 80% by 85%；40min~60min, the percentage by volume of mobile phase A by
20% is changed to 50%, and the percentage by volume of Mobile phase B is changed to 50% by 80%.
In wherein some embodiments, the flow velocity of the mobile phase is 0.8mL/min~1.2mL/min；The color
The column temperature for composing column is 25 DEG C~35 DEG C；The Detection wavelength used that measures is 210nm~250nm.
In wherein some embodiments, the organic solvent is the methanol solution that volumetric concentration is 70%~100%.
Compared with prior art, the present invention have it is following the utility model has the advantages that
Inventor is on the basis of permanent experience accumulation and after many experiments, select ferulic acid, Paeoniflorin, morroniside,
Loganin, which is used as, constructs finger-print referring to product, can not only characterize the quality of Zhong Yu decoction this classical dosage form well and
And the quality that its Modern preparations supports the beautiful soft extracts of essence kind, supports the beautiful granule of essence kind can also be characterized.In particular, cooperation is selected suitably
Chromatographic condition constructs finger-print, can not only qualitative, quantitatively characterizing Zhong Yu decoction, and characterization that can also be qualitative, quantitative
It supports the beautiful soft extracts of essence kind, support the beautiful granule of essence kind.
With the measuring method of this fingerprint map construction, it can not only make that Zhong Yu decoction standard decoction is qualitative, quantitative same stepping
Row, it is important to Zhong Yu decoction Modern preparations can also be suitable for simultaneously and support the beautiful soft extracts of essence kind, support the qualitative of the beautiful granule of essence kind
Quantitative test discloses the substance transmitting for supporting smart kind of jade side well.And the measuring method has easy, stable, precision height
And the features such as favorable reproducibility.
Detailed description of the invention
Fig. 1 is the finger-print and content (specificity test) map that the beautiful standard decoction of essence kind is supported in embodiment 1；Wherein,
Peak 6 is morroniside, and peak 7 is loganin, and peak 11 is Paeoniflorin, and peak 8 is 4,5-Dicaffeoylquinic acid, and peak 12 is ferulic acid；
Fig. 2 is the 9 batches of finger-prints and content map for supporting the beautiful standard decoction of essence kind in embodiment 1；
Fig. 3 is the reference fingerprint that the beautiful standard decoction of essence kind is supported in embodiment 1；
Fig. 4 is 9 batches of similarity evaluation results for supporting the beautiful standard decoction of essence kind in embodiment 1；
Fig. 5 is Precision test result stacking chart in embodiment 1；
Fig. 6 is repeated experiment result stacking chart in embodiment 1；
Fig. 7 is Intermediate precision test-difference personnel result stacking chart in embodiment 1；
Fig. 8 is Intermediate precision test-not same date result stacking chart in embodiment 1；
Fig. 9 is Intermediate precision test-difference instrument result stacking chart in embodiment 1；
Figure 10 is stability test result stacking chart in embodiment 1；
Figure 11 is ferulic acid standard curve in embodiment 1；
Figure 12 is Paeoniflorin standard curve in embodiment 1；
Figure 13 is morroniside standard curve in embodiment 1；
Figure 14 is loganin standard curve in embodiment 1；
Figure 15 is the experimental result of embodiment 2；
Figure 16 is the profiling results of comparative example 1；
Figure 17 is the profiling results of comparative example 2；
Figure 18 is the profiling results of comparative example 3；
Figure 19 is the profiling results of comparative example 4；
Figure 20 is the profiling results of comparative example 5；
Figure 21 is the profiling results of comparative example 6；
Figure 22 is the profiling results of comparative example 7.
Specific embodiment
It to facilitate the understanding of the present invention, below will be to invention is more fully described.But the present invention can be to be permitted
Mostly different form is realized, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes
It is more thorough and comprehensive to the understanding of the disclosure.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
Embodiment 1
1. instrument and reagent
1.1 instruments: electronic balance Mettler Toledo XP205DR (d=0.01mg), Mettler Toledo
MS204S (d=0.1mg), high-frequency digitally controlled ultrasonic cleaner (KQ-300TD, Kunshan Ultrasonic Instruments Co., Ltd.)
Simplicity UV water purification machine (Millipore), high performance liquid chromatograph (Agilent 1260), freeze drier (Germany
Christ, ALPHA2-4LD plus), Rotary Evaporators N-1200A (Shanghai EYELA Ai Lang Instrument Ltd.).
1.2 reagents: acetonitrile, phosphoric acid are chromatographically pure, and water is purified water, other reagents are that analysis is pure.
1.3 reagents: Paeoniflorin reference substance (National Institute for Food and Drugs Control, 110736-201539,110736-
201741), ferulic acid reference substance (National Institute for Food and Drugs Control, 110773-201313), loganin reference substance (China
Food and medicine examine and determine research institute, 111640-201005,111640-201707), (the Chinese food drug assay of morroniside reference substance
Research institute, 111998-201501,111998-201602), Rehmannia glutinosa, stir-baked RADIX PAEONIAE ALBA with vino, prepared RADIX ANGELICAE SINENSIS with yellow rice wine, wine-prepared fructus corni (Hubei day Ji Chinese medicine
Medicine materical crude slice Co., Ltd, Haozhou Huqiao Pharmaceutical Co., Ltd., Guangzhou Kang Sheng pharmaceutcal corporation, Ltd provides and Anhui another name for Sichuan Province Chinese medicinal material industry has
Limit company provide), superfine silica gel powder (Huzhou Zhanwang Pharmaceutical Co., Ltd.).
2. method and result
The preparation of 2.1 standard decoctions
Rehmannia glutinosa 60g, prepared RADIX ANGELICAE SINENSIS with yellow rice wine 30g, stir-baked RADIX PAEONIAE ALBA with vino 30g, wine-prepared fructus corni 30g, total 150g are taken, is soaked in water 30 minutes,
It decocts twice, for the first time plus water is 8 times of total weight, is decocted 1 hour, the filtration of 200 meshes, filtrate is spare；For the second time plus water is
8 times of total weight decoct 1 hour, and 200 meshes filtration, filtrate merges with first time filtrate, is concentrated under reduced pressure under the conditions of 50 DEG C,
Until forming inventory: after concentrate quality is the clear cream of 1:1~1:1.5,8% superfine silica gel powder is added, at -20 to -45 DEG C
Pre-freeze is lyophilized into powder under conditions of -80 DEG C, < 100Pa to get standard decoction freeze-dried powder.
With chemical composition content in Rehmannia glutinosa, prepared RADIX ANGELICAE SINENSIS with yellow rice wine, stir-baked RADIX PAEONIAE ALBA with vino and wine-prepared fructus corni for four factors, every kind of prepared slices of Chinese crude drugs have 3
A batch carries out L using this 3 batches as three levels9(34) orthogonal test, obtain 9 batches of freeze-dried powders.Medicine materical crude slice factor level table
It is shown in Table 1, positive quadraturing design test table is shown in Table 2.
1 Rehmannia glutinosa of table, prepared RADIX ANGELICAE SINENSIS with yellow rice wine, stir-baked RADIX PAEONIAE ALBA with vino and wine-prepared fructus corni medicine materical crude slice factor level table
2 positive quadraturing design test table of table
2.2 chromatographic condition
Chromatographic column: Phenomenex C18 (4.6 × 250mm, 5 μm)；Mobile phase: dense with volume using acetonitrile as mobile phase A
Degree is Mobile phase B for 0.1% phosphate aqueous solution, carries out gradient elution by the regulation in table 3；Column temperature: 25 DEG C；Flow velocity:
1.0mL/min；Detection wavelength: 240nm；Sample volume: 10 μ L.
3 eluent gradient elution requirement of table
| Time (min) | Acetonitrile (A) % | 0.1% phosphoric acid (B) % |
| 0~25 | 5~15 | 95~85 |
| 25~40 | 15~20 | 85~80 |
| 40~60 | 20~50 | 80~50 |
The preparation of 2.3 test solutions
The powder for taking standard decoction freeze-dried powder to obtain in right amount, it is finely ground, about 1g is taken, accurately weighed, precision is added plus 70% first
Alcohol 50mL, close plug, weighed weight, ultrasonic treatment (power 300W, frequency 40kHz) 30 minutes are taken out, are let cool, then weighed weight,
The weight that less loss is supplied with the methanol of 70% (percent by volume), shakes up, and filtration takes subsequent filtrate to get test solution.
The preparation of 2.4 mixed reference substance solutions
Accurately weighed ferulic acid, Paeoniflorin, morroniside, loganin reference substance respectively add 70% (volume basis after mixing
Than) mixing of every 1mL containing 12 μ g of ferulic acid, 42.11 μ g of Paeoniflorin, 40.29 μ g of morroniside, 50.64 μ g of loganin is made in methanol
Solution is to get mixed reference substance solution.
2.5 measuring method
It is accurate respectively to draw mixed reference substance solution and each 10 μ L of test solution, high performance liquid chromatograph is injected, efficiently
Liquid chromatography for measuring records chromatogram to get the finger-print and content of the beautiful standard decoction of feeding essence kind, sees Fig. 1.In Fig. 1,9
Number peak, No. 10 peaks and No. 11 peaks belong to stir-baked RADIX PAEONIAE ALBA with vino, and No. 12 peaks belong to prepared RADIX ANGELICAE SINENSIS with yellow rice wine, No. 2 peaks, No. 6 peaks, No. 7 peaks, No. 8 peaks and
No. 13 peaks belong to wine-prepared fructus corni, and the component content in Rehmannia glutinosa is extremely low to be pointed out.
The foundation of 2.6 reference fingerprints and similarity evaluation
Compare 9 batches of Zhong Yu decoction standard decoctions, based on shared peak occurrence rate 100%, it is determined that 14 shared peaks, by 9
It criticizes Zhong Yu decoction standard decoction and imports " similarity evaluation 2012 editions ", generate control fingerprint image
Spectrum, 9 batches of Zhong Yu decoction standard decoction similarities are 0.99 or more.See Fig. 2, Fig. 3, Fig. 4.
Ferulic acid, Paeoniflorin, morroniside, determination of loganin content in 2.7 9 batches of standard decoction freeze-dried powders
Every batch of standard decoction sample prepares two parts in parallel, and every part calculates asafoetide in standard decoction by external standard two-point method into two needles
The content (being averaged) of the index components such as acid, Paeoniflorin, morroniside, loganin, measurement result is shown in Table 4.
The content of ferulic acid, Paeoniflorin, morroniside, loganin in 49 batches of standard decoctions of table
3. fingerprint spectrum method is investigated
The test of 3.1 specificities
To investigate whether blank solvent and excipient micro-silica gel have interference, take test solution, mixing reference substance molten respectively
Liquid, blank solvent (70% methanol), excipient micro-silica gel solution are measured by method under " 2.2 chromatographic condition " item, record chromatography
Figure, measurement result are shown in Fig. 1.
The result shows that auxiliary material and blank solvent are noiseless.
3.2 precision test
It takes and supports beautiful 1 part of sample of the standard decoction of essence kind, it is accurate respectively by method preparation below " preparation of 2.3 test solutions " item
Same 10 μ L of test solution is drawn, continuous sample introduction 6 times, is measured by method under " 2.2 chromatographic condition " item, is recorded chromatogram, press
Similarity evaluation calculates its similarity, and similarity measurement result is shown in Fig. 5, table 5.
The result shows that similarity shows that instrument precision is good 1.000.
5 precision test similarity evaluation table of table
| Number | 1 | 2 | 3 | 4 | 5 | 6 | Reference fingerprint |
| 1 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| 2 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| 3 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| 4 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| 5 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| 6 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| Reference fingerprint | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
3.3 repetitive test
It takes and supports beautiful 6 parts of sample of the standard decoction of essence kind, it is accurate respectively by method preparation below " preparation of 2.3 test solutions " item
Same 10 μ L of test solution is drawn, is measured by method under " 2.2 chromatographic condition " item, chromatogram is recorded, by Chinese medicine chromatographic fingerprint
Map similarity evaluation system calculates its similarity, and similarity measurement result is shown in Fig. 6, table 6.
The result shows that similarity shows repeated good 1.000.
6 repetitive test similarity evaluation table of table
| Number | Repeatability 1 | Repeatability 2 | Repeatability 3 | Repeatability 4 | Repeatability 5 | Repeatability 6 | Reference fingerprint |
| Repeatability 1 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| Repeatability 2 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| Repeatability 3 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| Repeatability 4 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| Repeatability 5 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| Repeatability 6 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| Reference fingerprint | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
3.4 Intermediate precision
It takes with the beautiful standard decoction sample of the feeding essence kind of a batch, prepares by method below " preparation of 2.3 test solutions " item, exist respectively
Different time on different instruments, is measured by different personnel by method under " 2.2 chromatographic condition " item, chromatogram is recorded, by Chinese medicine
Chromatographic fingerprinting similarity evaluation system calculates its similarity, and similarity measurement result is shown in Fig. 7, Fig. 8, Fig. 9, table
7, table 8, table 9.
The result shows that similarity shows that Intermediate precision is good 0.999 or more.
The different personnel's similarity evaluation tables of table 7
| Different personnel | Liu | It is old | Reference fingerprint |
| Liu | 1.000 | 0.999 | 1.000 |
| It is old | 0.999 | 1.000 | 1.000 |
| Reference fingerprint | 1.000 | 1.000 | 1.000 |
The not same date similarity evaluation table of table 8
| Not same date | 20170823 | 20170803 | Reference fingerprint |
| 20170823 | 1.000 | 0.999 | 1.000 |
| 20170803 | 0.999 | 1.000 | 1.000 |
| Reference fingerprint | 1.000 | 1.000 | 1.000 |
The different instrument similarity evaluation tables of table 9
| Different instruments | waters | agilent | Reference fingerprint |
| waters | 1.000 | 0.997 | 0.999 |
| agilent | 0.997 | 1.000 | 0.999 |
| Reference fingerprint | 0.999 | 0.999 | 1.000 |
3.5 stability test
It takes and supports beautiful 1 part of sample of the standard decoction of essence kind, prepared by method below " preparation of 2.3 test solutions " item, respectively at 0,
2,4,8,16,24,36,48,60,72h, it is measured by method under " 2.2 chromatographic condition " item, records chromatogram, refer to by Chinese medicine chromatography
Line map similarity evaluation system calculates its similarity, and similarity measurement result is shown in Figure 10, table 10.
The result shows that similarity shows that test solution is good in 72h internal stability 1.000.
10 stability similarity evaluation table of table
4 content assaying methods are investigated
The test of 4.1 specificities
With measuring under " 3.1 " item, chromatogram is recorded.The result shows that blank solvent, excipient micro-silica gel solution with asafoetide
The corresponding retention time of acid, Paeoniflorin, morroniside, loganin does not have chromatographic peak.
The result shows that blank solvent and excipient micro-silica gel are to the measurement of ferulic acid, Paeoniflorin, morroniside, loganin without dry
It disturbs, the content of ferulic acid in this product, Paeoniflorin, morroniside, loganin is measured with specificity with this law.
The investigation of 4.2 linear relationships
Accurately weighed ferulic acid, Paeoniflorin, morroniside, loganin reference substance respectively, after mixing plus 70% methanol dissolves, i.e.,
Mixed reference substance solution is obtained, contains 12.00 μ g of ferulic acid, 42.11 μ g of Paeoniflorin, morroniside 40.29 in mixing control described in every 1mL
μ g, 50.64 μ g of loganin.It is accurate respectively to draw above-mentioned 0.5 μ L of reference substance solution, 2 μ L, 5 μ L, 8 μ L, 10 μ L, 12 μ L, 15 μ L,
It is measured by method under " 2.2 chromatographic condition " item, records chromatogram.With sample volume (mg) for abscissa, peak area is ordinate, is drawn
Standard curve processed is shown in Table 11, table 12, table 13, table 14, Figure 11, Figure 12, Figure 13, Figure 14.Ferulic acid regression equation is y=3,
110.5432x+0.6280, R2=0.9997；Paeoniflorin regression equation is y=1,104.5941x-3.7299, R2=0.9999；
Morroniside regression equation is y=1,669.1956x+2.2166, R2=0.9998；Loganin regression equation is y=1,
632.6540x+3.3200, R2=0.9996.
The result shows that ferulic acid is in 0.0060mg~0.1800mg, Paeoniflorin in 0.0211mg~0.6317mg, morroniside
It is linear good within the scope of 0.0253mg~0.7596mg in 0.0201mg~0.6044mg, loganin.
Investigation result-ferulaic acid content of 11 linear relationship of table
Investigation result-paeoniflorin content of 12 linear relationship of table
Investigation result-morroniside content of 13 linear relationship of table
Investigation result-Determination of Loganin of 14 linear relationship of table
4.3 precision test
With being measured under " 3.2 " item, chromatogram is recorded, peak area is calculated, the results are shown in Table 15, table 16, table 17, table
18, as a result each ingredient RSD < 2%, shows that instrument precision is good.
15 Precision test results of table-ferulaic acid content
16 Precision test results of table-paeoniflorin content
17 Precision test results of table-morroniside content
18 Precision test results of table-Determination of Loganin
4.4 repetitive test
With being measured under " 3.3 " item, chromatogram is recorded, peak area is calculated, the results are shown in Table 19, RSD < 2%, illustrates this
The repeatability of method is good.
19 repetitive test result (n=6) of table
| Number | 1 | 2 | 3 | 4 | 5 | 6 | Average value | RSD (%) |
| Ferulaic acid content (mg/g) | 0.179 | 0.184 | 0.182 | 0.186 | 0.181 | 0.183 | 0.183 | 1.33 |
| Paeoniflorin content (mg/g) | 6.055 | 6.152 | 6.242 | 6.321 | 6.352 | 6.209 | 6.222 | 1.76 |
| Morroniside content (mg/g) | 3.307 | 3.379 | 3.416 | 3.469 | 3.473 | 3.399 | 3.407 | 1.82 |
| Determination of Loganin (mg/g) | 1.631 | 1.665 | 1.81 | 1.708 | 1.713 | 1.672 | 1.678 | 1.80 |
4.5 stability test
With being measured under " 3.4 " item, chromatogram is recorded, peak area is calculated, measurement result is shown in Table 20.Ferulic acid, Chinese herbaceous peony
The RSD of medicine glycosides, morroniside and loganin is respectively 1.43%, 0.69%, 1.28% and 0.81%, shows test solution 72
Hour internal stability is good.
20 stability test result of table
4.6 accuracy test
Using sample-adding absorption method, this product powder about 0.26g is taken, it is accurately weighed (totally 9 parts), it splits in stuffed conical flask, point
It is accurate that mixed reference substance solution 1ml, 2ml, 3ml (each 3 parts) are added, then 70% methanol 50mL is added in precision respectively, close plug claims
Determine weight, ultrasonic treatment (power 250W, frequency 40kHz) 30 minutes is taken out, lets cool, then weighed weight, supplied with 70% methanol
The weight of less loss, shakes up, filtration, precision draw 10 μ l of subsequent filtrate, inject liquid chromatograph, measurement to get.The results are shown in Table 21,
Table 22, table 23, table 24, ferulic acid, Paeoniflorin, morroniside and loganin average recovery rate be respectively 103.74%,
97.63%, 101.04%, 103.50%, RSD is respectively 3.48%, 2.11%, 2.01%, 1.60%, shows that this method is accurate
Degree is good.
21 accuracy test result of table-ferulic acid
22 accuracy test result of table-Paeoniflorin
23 accuracy test result of table-morroniside
24 accuracy test result of table-loganin
Embodiment 2
The finger-print that the present embodiment is prepared using embodiment 1 examines the unqualified Zhong Yu decoction agent that raw material lacks
It surveys.
Referring to 2.1 method of embodiment 1, preparing failed test sample 1, (composition of raw materials is Rehmannia glutinosa: prepared RADIX ANGELICAE SINENSIS with yellow rice wine: wine-prepared fructus corni
=2:1:1), failed test sample 2 (composition of raw materials is Rehmannia glutinosa: stir-baked RADIX PAEONIAE ALBA with vino: wine-prepared fructus corni=2:1:1), 3 (raw material of failed test sample
Formula be Rehmannia glutinosa: prepared RADIX ANGELICAE SINENSIS with yellow rice wine: stir-baked RADIX PAEONIAE ALBA with vino=2:1:1), (composition of raw materials is prepared RADIX ANGELICAE SINENSIS with yellow rice wine to failed test sample 4: stir-baked RADIX PAEONIAE ALBA with vino: wine-prepared fructus corni
=1:1:1), and referring to 2.3 method of embodiment 1 prepare failed test sample test solution, referring to the 2.4 of embodiment 1
Method prepares mixed reference substance solution, and 2.2 chromatographic condition referring next to embodiment 1 and 2.5 measuring method are detected.With
1 finger-print of above-described embodiment detects the above-mentioned rejected product, records chromatogram (see Figure 15) and imports Chinese medicine chromatography
Similarity evaluation system software compares trace analysis with what embodiment 1 obtained, calculates similarity, as a result as shown in table 25 below.From
As a result as can be seen that the similarity of rejected product is respectively less than 0.9.Show that 1 finger-print of embodiment can be used as Zhong Yu decoction
The quality of agent controls and evaluation index.
Table 25
Embodiment 3
The finger-print that the present embodiment is prepared using embodiment 1 detects the beautiful soft extracts of feeding essence kind.
The preparation of test solution: taking and support the beautiful soft extracts of essence kind about 1g, and accurately weighed, precision is added plus 70% methanol 50mL,
Close plug, weighed weight, ultrasonic treatment (power 300W, frequency 40kHz) 30 minutes are taken out, are let cool, then weighed weight, with 70%
The methanol of (percent by volume) supplies the weight of less loss, shakes up, and filtration takes subsequent filtrate to get test solution.Remaining operation side
Method is the same as embodiment 1.
Finger-print is the results show that it is compared with reference fingerprint, and 14 shared peaks occur, and similarity exists
0.95 or more.The result shows that the finger-print that embodiment 1 constructs, which can also be used to Quality Control, supports the beautiful soft extracts of essence kind.
Embodiment 4
The finger-print that the present embodiment is prepared using embodiment 1 detects the beautiful granule of feeding essence kind.
The preparation of test solution: it takes and supports the beautiful granule of essence kind about 1g, accurately weighed, precision is added plus 70% methanol
50mL, close plug, weighed weight, ultrasonic treatment (power 300W, frequency 40kHz) 30 minutes are taken out, are let cool, then weighed weight, use
The methanol of 70% (percent by volume) supplies the weight of less loss, shakes up, and filtration takes subsequent filtrate to get test solution.Remaining behaviour
Make method with embodiment 1.
Finger-print is the results show that it is compared with reference fingerprint, and 14 shared peaks occur, and similarity exists
0.95 or more, illustrate that the finger-print that embodiment 1 constructs can also be used to the beautiful granule of the feeding essence kind of Quality Control.
Comparative example 1
This comparative example is the comparative example of embodiment 1, compared with Example 1, in place of essential difference includes that chromatographic condition is different.
Specific chromatographic condition is as follows:
Chromatographic column: Phenomenex C18 (4.6 × 250mm, 5 μm)；Mobile phase: dense with volume using acetonitrile as mobile phase A
Degree is Mobile phase B for 0.1% phosphate aqueous solution, and the regulation according to the form below carries out isocratic elution (referring to table 26)；Column temperature: 25
℃；Flow velocity: 1mL/min；Detection wavelength: 240nm；Sample volume: 10 μ L.
26 mobile phase isocratic condition of table
| Time (min) | Acetonitrile (A) % | 0.1% phosphoric acid (B) % |
| 0~50 | 13 | 87 |
The finger-print result See Figure 16 of this comparative example building, in figure, 1: morroniside；2: loganin；3: Paeoniflorin；4:
Ferulic acid.The results show that morroniside Interference Peaks are more, it is difficult to individually separate it.
Comparative example 2
This comparative example is the comparative example of embodiment 1, compared with Example 1, in place of essential difference includes that chromatographic condition is different.
Specific chromatographic condition is as follows:
Chromatographic column: Phenomenex C18 (4.6 × 250mm, 5 μm)；Mobile phase: dense with volume using acetonitrile as mobile phase A
Degree is Mobile phase B for 0.1% phosphate aqueous solution, and the regulation according to the form below 27 carries out gradient elution；Column temperature: 25 DEG C；Flow velocity:
1mL/min；Detection wavelength: 240nm；Sample volume: 10 μ L.
The finger-print the result is shown in Figure 17 of this comparative example building, in figure, 1: morroniside；2: loganin；3: Paeoniflorin；4: Ah
Wei's acid.Morroniside Interference Peaks are more as the result is shown, it is difficult to individually separate it.
27 eluent gradient elution requirement of table
| Time (min) | Acetonitrile (A) % | 0.1% phosphoric acid (B) % |
| 0~10 | 10~12 | 90~88 |
| 10~15 | 12~14 | 88~86 |
| 15~30 | 14~20 | 86~80 |
| 30~40 | 20~38 | 80~62 |
Comparative example 3
This comparative example is the comparative example of embodiment 1, compared with Example 1, in place of essential difference includes that chromatographic condition is different.
Specific chromatographic condition is as follows:
Chromatographic column: Phenomenex C18 (4.6 × 250mm, 5 μm)；Mobile phase: dense with volume using acetonitrile as mobile phase A
Degree is Mobile phase B for 0.1% phosphate aqueous solution, and the regulation according to the form below 28 carries out gradient elution；Column temperature: 25 DEG C；Flow velocity:
1mL/min；Detection wavelength: 240nm；Sample volume: 10 μ L.
The finger-print result of this comparative example building is shown in 18 figures, in figure, 1: morroniside；2: loganin；3: Paeoniflorin；4: Ah
Wei's acid.Morroniside Interference Peaks are more as the result is shown, it is difficult to individually separate it.
28 eluent gradient elution requirement of table
| Time (min) | Acetonitrile (A) % | 0.1% phosphoric acid (B) % |
| 0~25 | 10~14 | 90~86 |
| 25~60 | 14~26 | 86~74 |
Comparative example 4
This comparative example is the comparative example of embodiment 1, compared with Example 1, in place of essential difference includes that chromatographic condition is different.
Specific chromatographic condition is as follows:
Chromatographic column: Phenomenex C18 (4.6 × 250mm, 5 μm)；Mobile phase: dense with volume using acetonitrile as mobile phase A
Degree is Mobile phase B for 0.1% phosphate aqueous solution, and the regulation according to the form below 29 carries out gradient elution；Column temperature: 25 DEG C；Flow velocity:
1mL/min；Detection wavelength: 240nm；Sample volume: 10 μ L.
The finger-print the result is shown in Figure 19 of this comparative example building, in figure, 1: morroniside；2: loganin；3: Paeoniflorin；4: Ah
Wei's acid.Morroniside Interference Peaks are more as the result is shown, it is difficult to individually separate it.
29 eluent gradient elution requirement of table
Comparative example 5
This comparative example is the comparative example of embodiment 1, compared with Example 1, in place of essential difference includes that chromatographic condition is different.
Specific chromatographic condition is as follows:
Chromatographic column: Phenomenex C18 (4.6 × 250mm, 5 μm)；Mobile phase: dense with volume using acetonitrile as mobile phase A
Degree is Mobile phase B for 0.1% phosphate aqueous solution, and the regulation according to the form below 30 carries out gradient elution；Column temperature: 25 DEG C；Flow velocity:
1mL/min；Detection wavelength: 240nm；Sample volume: 10 μ L.
The finger-print result of this comparative example building is shown in Figure 20, in figure, 1: morroniside；2: loganin；3: Paeoniflorin；4: Ah
Wei's acid.Morroniside Interference Peaks are more as the result is shown, it is difficult to individually separate it.
30 eluent gradient elution requirement of table
| Time (min) | Acetonitrile (A) % | 0.1% phosphoric acid (B) % |
| 0~25 | 10~14 | 90~86 |
| 25~46 | 14~27 | 86~73 |
| 46~60 | 27~85 | 73~15 |
Comparative example 6
This comparative example is the comparative example of embodiment 1, compared with Example 1, in place of essential difference includes the elution ladder used
Degree is different.Specific chromatographic condition is as follows:
Chromatographic column: Phenomenex C18 (4.6 × 250mm, 5 μm)；Mobile phase: dense with volume using acetonitrile as mobile phase A
Degree is Mobile phase B for 0.1% phosphate aqueous solution, and the regulation according to the form below 31 carries out gradient elution；Column temperature: 25 DEG C；Flow velocity:
0.8mL/min；Detection wavelength: 240nm；Sample volume: 10 μ L.
This comparative example constructs finger-print using the chromatographic condition, and supports smart kind of jade side's soft extracts for detecting.This comparative example
The finger-print result of building is shown in Figure 21, wherein 1: morroniside；2: loganin；3: Paeoniflorin；4: ferulic acid；5: verbascose
Glycosides.Morroniside Interference Peaks are more as the result is shown, it is difficult to individually separate it.Meanwhile inventors have found that building finger-print with
The map similarity for supporting essence kind of jade side's soft extracts differs greatly, and cannot be used for Quality Control at all and supports smart kind of jade side's soft extracts.
Table 31, eluent gradient elution requirement
| Time (min) | Acetonitrile (A) % | 0.1% phosphoric acid (B) % |
| 0~25 | 10~14 | 90~86 |
| 25~46 | 14~27 | 86~73 |
| 46~50 | 27~80 | 73~20 |
Comparative example 7
This comparative example of the finger-print of this comparative example building is the comparative example of embodiment 1, compared with Example 1, main poor
Place does not include the gradient difference used.Specific chromatographic condition is as follows:
Chromatographic column: Phenomenex C18 (4.6 × 250mm, 5 μm)；Mobile phase: dense with volume using acetonitrile as mobile phase A
Degree is Mobile phase B for 0.1% phosphate aqueous solution, and the regulation according to the form below 32 carries out gradient elution；Column temperature: 25 DEG C；Flow velocity:
1.0mL/min；Detection wavelength: 240nm；Sample volume: 10 μ L.
This comparative example constructs finger-print using the chromatographic condition, and supports smart kind of jade side's granule for detecting.This comparison
The finger-print result See Figure 22 of example building, 1 in figure: morroniside；2: loganin；3: Paeoniflorin；4: ferulic acid.As the result is shown
Morroniside Interference Peaks are more, it is difficult to individually separate it.Meanwhile inventors have found that the finger-print of building and feeding smart kind of jade side
The map similarity of granule differs greatly, and cannot be used for Quality Control at all and supports smart kind of jade side's soft extracts.
32 eluent gradient elution requirement of table
| Time (min) | Acetonitrile (A) % | 0.1% phosphoric acid (B) % |
| 0~30 | 5~25 | 95~75 |
| 30~60 | 25~80 | 75~20 |
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. the construction method of the finger-print of the beautiful prescription of breeding essence kind, which is characterized in that the construction method includes the following steps:
Test solution preparation: resting the beautiful decoction of essence kind and be prepared into freeze-dried powder, the freeze-dried powder is dissolved in organic solvent, is filtered,
Obtain test solution；
Reference substance solution preparation: ferulic acid, Paeoniflorin, morroniside, loganin reference substance are dissolved in organic solvent, it is molten to obtain reference substance
Liquid；
The building of finger-print: drawing the test solution, reference substance solution, and injection high performance liquid chromatograph measurement obtains
To the beautiful prescription finger-print of feeding essence kind with common characteristic peaks.
2. the construction method of the finger-print of the beautiful prescription of feeding essence kind according to claim 1, which is characterized in that the measurement
The chromatographic condition of use includes:
Chromatographic column: using octadecylsilane chemically bonded silica as filler；
Mobile phase: using acetonitrile as mobile phase A, the phosphate aqueous solution for being 0.08%~0.12% using volumetric concentration is Mobile phase B；
Gradient elution mode: the percentage by volume of 0min~25min, mobile phase A are changed to 15% by 5%, the volume of Mobile phase B
Percentage is changed to 85% by 95%；Mobile phase is changed to by 25min~40min, the percentage by volume of mobile phase A by 15%
20%, the percentage by volume of Mobile phase B is changed to 80% by 85%；40min~60min, the percentage by volume of mobile phase A by
20% is changed to 50%, and the percentage by volume of Mobile phase B is changed to 50% by 80%.
3. the construction method of the finger-print of the beautiful prescription of feeding essence kind according to claim 2, which is characterized in that the stream
The flow velocity of dynamic phase is 0.8mL/min~1.2mL/min；The column temperature of the chromatographic column is 25 DEG C~35 DEG C；The measurement uses
Detection wavelength be 210nm~250nm.
4. the construction method of the finger-print of the beautiful prescription of feeding essence kind according to any one of claims 1 to 3, feature exist
In the organic solvent is the methanol solution that volumetric concentration is 70%~100%.
5. the construction method of the finger-print of the beautiful prescription of feeding essence kind according to any one of claims 1 to 3, feature exist
In the freeze-dried powder 0.5g~1g is added in organic solvent described in every 25mL~50mL.
6. the construction method of the finger-print of the beautiful prescription of feeding essence kind according to any one of claims 1 to 3, feature exist
In, in contrast solution described in every 1mL containing 0.6 μ g of μ g~24 of ferulic acid, 2.1 μ g of μ g~84.2 of Paeoniflorin, 2.0 μ g of morroniside~
80.6 μ g, 2.5 μ of μ g~101.3 g of loganin.
7. the measuring method of the beautiful prescription of breeding essence kind, which is characterized in that the measuring method includes the following steps:
Test solution preparation: the feeding beautiful prescription of essence kind to be measured is dissolved in organic solvent, filters, obtains test solution；
Reference substance solution preparation: ferulic acid, Paeoniflorin, morroniside, loganin reference substance are dissolved in organic solvent, it is molten to obtain reference substance
Liquid；
Test solution measurement: drawing the test solution, reference substance solution, and injection high performance liquid chromatograph is surveyed
It is fixed, obtain the map of the beautiful prescription of feeding essence kind to be measured；What the map and claim 1 for comparing the feeding beautiful prescription of essence kind to be measured constructed
The peak area at the relative retention time at each peak and/or each peak in finger-print, complete to the qualitative of the feeding beautiful prescription of essence kind to be measured and/
Or quantitative determination.
8. the measuring method of the beautiful prescription of feeding essence kind according to claim 7, which is characterized in that the chromatography that the measurement uses
Condition includes:
Chromatographic column: using octadecylsilane chemically bonded silica as filler；
Mobile phase: using acetonitrile as mobile phase A, the phosphate aqueous solution for being 0.08%~0.12% using volumetric concentration is Mobile phase B；
Gradient elution mode: the percentage by volume of 0min~25min, mobile phase A are changed to 15% by 5%, the volume of Mobile phase B
Percentage is changed to 85% by 95%；Mobile phase is changed to by 25min~40min, the percentage by volume of mobile phase A by 15%
20%, the percentage by volume of Mobile phase B is changed to 80% by 85%；40min~60min, the percentage by volume of mobile phase A by
20% is changed to 50%, and the percentage by volume of Mobile phase B is changed to 50% by 80%.
9. the measuring method of the beautiful prescription of feeding essence kind according to claim 8, which is characterized in that the flow velocity of the mobile phase
For 0.8mL/min~1.2mL/min；The column temperature of the chromatographic column is 25 DEG C~35 DEG C；The Detection wavelength that the measurement uses
For 210nm~250nm.
10. the measuring method of the beautiful prescription of feeding essence kind according to any one of claims 7 to 9, which is characterized in that described has
Solvent is the methanol solution that volumetric concentration is 70%~100%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413443A (en) * | 2020-05-08 | 2020-07-14 | 四川新绿色药业科技发展有限公司 | Characteristic spectrum, construction method and identification method of angelica sinensis and decoction pieces thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958039A (en) * | 2006-11-24 | 2007-05-09 | 王建兴 | Preparation of Chinese traditional medicine for treating cardiovascular disease, and cerebrovascular disease |
| CN101991661A (en) * | 2009-08-19 | 2011-03-30 | 中国药品生物制品检定所 | Method for detecting Chinese patent drug containing at least two of white paeony root, ginseng, salvia miltiorrhiza, sweet wormwood, liquorice and angelica sinensis |
| CN102028840A (en) * | 2009-09-28 | 2011-04-27 | 中国药品生物制品检定所 | Ultrahigh pressure liquid phase detection method for Chinese patent medicine |
| CN107764924A (en) * | 2016-08-19 | 2018-03-06 | 江苏康缘药业股份有限公司 | The detection method of active ingredient in asthma particle |
-
2018
- 2018-10-22 CN CN201811229630.0A patent/CN109507310B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958039A (en) * | 2006-11-24 | 2007-05-09 | 王建兴 | Preparation of Chinese traditional medicine for treating cardiovascular disease, and cerebrovascular disease |
| CN101991661A (en) * | 2009-08-19 | 2011-03-30 | 中国药品生物制品检定所 | Method for detecting Chinese patent drug containing at least two of white paeony root, ginseng, salvia miltiorrhiza, sweet wormwood, liquorice and angelica sinensis |
| CN102028840A (en) * | 2009-09-28 | 2011-04-27 | 中国药品生物制品检定所 | Ultrahigh pressure liquid phase detection method for Chinese patent medicine |
| CN107764924A (en) * | 2016-08-19 | 2018-03-06 | 江苏康缘药业股份有限公司 | The detection method of active ingredient in asthma particle |
Non-Patent Citations (4)
| Title |
|---|
| HORNG-LIANG LAY 等: "Simultaneous Analysis of Nine Components in "Byi-Liang-Tang" Preparation by High Performan Liquid Chromatography", 《JOURNAL OF FOOD AND DRUG ANALYSIS》 * |
| 李龙 等: "养精种玉煎膏的HPLC指纹图谱研究", 《中药新药与临床药理》 * |
| 王岩 等: "养精种玉汤正丁醇部位的HPLC指纹图谱研究", 《中成药》 * |
| 马红霞 等: "养精种玉汤乙酸乙酯部位的HPLC指纹图谱研究", 《中国药房》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413443A (en) * | 2020-05-08 | 2020-07-14 | 四川新绿色药业科技发展有限公司 | Characteristic spectrum, construction method and identification method of angelica sinensis and decoction pieces thereof |
| CN111413443B (en) * | 2020-05-08 | 2022-03-22 | 四川新绿色药业科技发展有限公司 | Characteristic spectrum, construction method and identification method of angelica sinensis and decoction pieces thereof |
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