CN109884222A - A kind of HPLC fingerprint of Sabia parviflora Wall.ex Roxb - Google Patents
A kind of HPLC fingerprint of Sabia parviflora Wall.ex Roxb Download PDFInfo
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- CN109884222A CN109884222A CN201910044474.9A CN201910044474A CN109884222A CN 109884222 A CN109884222 A CN 109884222A CN 201910044474 A CN201910044474 A CN 201910044474A CN 109884222 A CN109884222 A CN 109884222A
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Abstract
The invention discloses a kind of HPLC fingerprints of Sabia parviflora Wall.ex Roxb.This method has easy, stable, precision height, high repeatability and other advantages；It more can also comprehensively reflect the type and quantity of contained chemical component in Sabia parviflora Wall.ex Roxb with this method, and then whole description and evaluation are carried out to its quality.And the Sabia parviflora Wall.ex Roxb finger-print chemical component that is detected with this method is relatively more, each characteristic peak height ratio is moderate, baseline is more steady, and separating degree and peak shape are good, and column effect is high.
Description
Technical field
The present invention relates to a kind of HPLC fingerprints of Sabia parviflora Wall.ex Roxb, belong to the field of drug technology.
Background technique
Traditional Chinese medicine fingerprint is a kind of synthesis, and quantifiable identification of means, it is built upon chemical composition of Chinese materia medica system
On the basis of research, it is mainly used for evaluating authenticity, Optimality and the stability of Chinese medicine and Chinese materia medica preparation semi-manufactured goods quality.
Chinese medicine and its preparation are multi-component complex system, therefore evaluate its quality and can should be provided to enrich and be reflected using adaptable therewith
The detection method of other information, establishing traditional Chinese medicine fingerprint more will comprehensively reflect contained chemical component in Chinese medicine and its preparation
Type and quantity, and then whole description and evaluation are carried out to drug quality.On this basis, it is learned if further carrying out spectrum effect
Research, can be such that traditional Chinese medicine quality really combines with its drug effect, help to illustrate Mechanism of TCM.
Sabia parviflora Wall.ex Roxb Sabia parviflora Wall.ex Roxb. is Sabiaceae Sabiaceae fresh breeze Calamus
Sabia plant is the common drug of the diseases such as the national treatment hepatitis such as Miao in Guizhou, Bouyei, rheumatic arthralgia, traumatic injury.
Modern research shows that Sabia parviflora Wall.ex Roxb and belonging to various plants and mainly containing alkaloids, flavonoids and triterpenes components, have very
Good antiviral, liver protection, drop enzyme, it is anti-inflammatory the effects of.In recent years, author is in state natural sciences fund, Guizhou Province's one stream subject
Sabia parviflora Wall.ex Roxb and its congener have been carried out under the subsidies of projects such as construction and reflected including resource investigation, introducing and planting, crude drug
The further investigation of fixed, quality of medicinal material, chemical component, pharmacological effect etc., discovery Sabia parviflora Wall.ex Roxb exploitation benefit with higher
With value, but the research of quality control aspect is also weaker.Have in terms of quality control and identification in view of traditional Chinese medicine fingerprint
There is outstanding advantage, author team is right on the basis of carrying out system research to fresh breeze Calamus resources of medicinal plant, chemical component etc.
The chemical fingerprint of Sabia parviflora Wall.ex Roxb has made intensive studies, and research achievement is the present invention.
Summary of the invention
Present invention aims at provide a kind of HPLC fingerprint of Sabia parviflora Wall.ex Roxb medicinal material.This method tool
There are easy, stable, precision height, high repeatability and other advantages；It more can also comprehensively reflect institute in Sabia parviflora Wall.ex Roxb with this method
Type and quantity containing chemical component, and then whole description and evaluation are carried out to its quality.And the little Hua detected with this method
Sabia japonica finger-print chemical component is relatively more, each characteristic peak height ratio is moderate, and baseline is more steady, separating degree and peak shape
Good, column effect is high.
In order to solve the above technical problems, the present invention adopts the following technical scheme that realization: a kind of HPLC of Sabia parviflora Wall.ex Roxb refers to
Line map method for building up, comprising the following steps:
(1) preparation of mixed reference substance solution: respectively precision weigh Quercetin -3-O- gentiobioside with cape jasmine,
Camellianoside, Tsubakioside A, kaempferol-3-O-rutinoside, the control of Isorhamnetin -3-O- rutinoside
Product, add 70% ethanol solution dissolve, shake up, be made Quercetin -3-O- gentiobioside with cape jasmine mass concentration be 0.0625mg/mL,
Camellianoside mass concentration is 0.250mg/mL, Tsubakioside A mass concentration is 0.0675mg/mL, kaempferia galamga
Phenol -3-O- rutinoside mass concentration is 0.0625mg/mL, Isorhamnetin -3-O- rutinoside mass concentration is 0.0500mg/
The mixed reference substance solution of mL；
(2) preparation of test solution: accurately weighed Sabia parviflora Wall.ex Roxb powder 1g, precision plus the dissolution of 70% ethanol solution,
Weighed weight, ultrasonic extraction are let cool, and are mended weight with 70% ethanol solution, are shaken up, filter, 0.45 μm of organic miillpore filter of filtrate
Filtering to get；
(3) chromatographic condition that finger-print is established: chromatographic column: Thermo Accucore-C18, 150 × 4.6mm, 2.6 μm；
Mobile phase: 30% tetrahydrofurfuryl carbinol solution is A phase, and acetonitrile is B phase, and 0.1% phosphate aqueous solution is C phase；Gradient elution, detection
Wavelength is 360nm, flow velocity 1mL/min, 30 DEG C of column temperature, 10 μ L of sample volume；Record spectrogram obtains Sabia parviflora Wall.ex Roxb medicinal material
HPLC finger-print；
(4) according to the method for above-mentioned offer, its HPLC the confirmation of standard fingerprint spectrogram: is established to multiple batches of Sabia parviflora Wall.ex Roxb
Finger-print is compared by analysis and 15 shared peaks has been determined, these shared peaks constitute the fingerprint characteristic of Sabia parviflora Wall.ex Roxb, is built
Common pattern is found, the standard finger-print as Sabia parviflora Wall.ex Roxb medicinal material.
In the HPLC fingerprint of Sabia parviflora Wall.ex Roxb above-mentioned, the test solution is prepared: accurate
Weighed Sabia parviflora Wall.ex Roxb powder 1g, sets in 50mL stuffed conical flask, precision plus 70% ethanol solution 15mL, weighed weight, ultrasound
60min is extracted, is let cool, weight is mended with 70% ethanol solution, shakes up, filter, 0.45 μm of organic filtering with microporous membrane of filtrate, i.e.,
?.
In the HPLC fingerprint of Sabia parviflora Wall.ex Roxb above-mentioned, when ultrasonic extraction, power 100W, frequency is
80Hz。
In the HPLC fingerprint of Sabia parviflora Wall.ex Roxb above-mentioned, when gradient elution, gradient elution program is: 0-
The B of the A of 5min:5% → 12% and 3% → 6%；The B of the A of 5-15min:12% → 10% and 6% → 8%；15-20min:
The B of 10% → 20% A and 8% → 10%；The B of the A of 20-35min:20% → 53% and 10% → 28%；35-45min:
The B of 53% A and 28%；The B of the A of 45-50min:53% → 70% and 28% → 30%；The A of 50-60min:70% → 65%
With 30% → 35% B.
In the HPLC fingerprint of Sabia parviflora Wall.ex Roxb medicinal material above-mentioned, in 15 shared peaks, No. 1 peak is
Quercetin -3-O- gentiobioside with cape jasmine, No. 2 peaks are Camellianoside, and No. 3 peaks are Tsubakioside A, and No. 4 peaks are kaempferia galamga
Phenol -3-O- rutinoside, No. 6 peaks are Isorhamnetin -3-O- rutinoside.
In the HPLC fingerprint of Sabia parviflora Wall.ex Roxb above-mentioned, 15 shared peaks, with No. 6 different sandlwoods in peak
Element -3-O- rutinoside is referring to peak, and relative retention time is respectively 0.444-0.447,0.515-0.518,0.714-
0.719、0.831-0.833、0.943-0.945、1.000、1.107-1.117、1.551-1.557、1.629-1.635、
1.646-1.653、1.664-1.671、1.776-1.784、1.804-1.813、2.250-2.260、2.282-2.292。
Inventor has carried out a large amount of experiment, is the research of detection method of the present invention below.
Experimental example: the HPLC finger-print research of Sabia parviflora Wall.ex Roxb
1 instrument and reagent
1.1 instrument
Thermo UltiMate-3000 type high performance liquid chromatograph, DAD detector (German Thermo company)；AG135
Type electronic balance (Mettler-Toledo company, Switzerland)；KQ-500DE type numerical control ultrasonic cleaner (city of Kunshan's ultrasonic instrument
Co., Ltd)；Thermo Hytimate-C18(150 × 4.6mm, 2.6 μm).
1.2 reagent
Methanol (U.S. world Co., Ltd, chromatographically pure.Sinopharm Chemical Reagent Co., Ltd. analyzes pure)；Acetonitrile (beauty
World Co., Ltd, state, chromatographically pure)；Tetrahydrofuran (Tianjin great Mao chemical reagent factory, chromatographically pure)；Ethyl alcohol (Tianjin richness space
Fine Chemical Co., Ltd analyzes pure)；Phosphoric acid (Chongqing Chuan Dong Chemical Co., Ltd. analyzes pure)；Formic acid (Tianjin technicalization
Reagent Co., Ltd is learned, is analyzed pure)；Experimental water is double distilled water.
Quercetin -3-O- gentiobioside with cape jasmine, Camellianoside, Tsubakioside A, Kaempferol -3-O- rutinose
Glycosides, Isorhamnetin -3-O- rutinoside, the above reference substance pass through ODS-A-HG C18Reversed chromatographic column and Ailgent
The equal separation workmanship art of 1100 type, half preparation solution, the monomeric compound voluntarily separated from Sabia parviflora Wall.ex Roxb stem and leaf, in conjunction with1H-
NMR and13The spectral datas such as C-NMR identify each compound structure, are calculated using HPLC areas of peak normalization method, and mass fraction is equal
Greater than 98%, for assay reference substance use.
The source of 1.3 test samples
Experiment is picked up from person by author in provinces and regions such as Guizhou, Yunnan, Guangxi with sample, and through Guizhou university of TCM grandson
Celebrating culture and education, which is awarded, is accredited as Sabiaceae (Sabiaceae) plant Sabia parviflora Wall.ex Roxb (Sabia parviflora
Wall.ex.Roxb. leaf), plant voucher specimen are stored in Guizhou university of TCM crude drug laboratory.Sample message is detailed in table
1。
1 Sabia parviflora Wall.ex Roxb sample source information of table
2 methods and result
The determination of 2.1 chromatographic conditions
Chromatographic column: Thermo Accucore-C18(150×4.6mm,2.6μm)；Detection wavelength: 360nm；Column temperature: 30 DEG C；
Sample volume: 10 μ L；Flow velocity 1.0mL/min；Mobile phase: 30% tetrahydrofurfuryl carbinol solution-acetonitrile -0.1% phosphate aqueous solution ladder
Degree elution, elution program are shown in Table 2.
2 eluent gradient elution program of table
The preparation of 2.2 test solutions
Sample powder about 1g is taken, it is accurately weighed, it sets in 50mL stuffed conical flask, precision plus 70% ethanol solution 15mL claim
Determining weight, ultrasonic extraction (power 100W, frequency 80Hz) 60min is let cool, and weight is mended with 70% ethanol solution, is shaken up, is filtered, filter
Liquid with 0.45 μm of organic filtering with microporous membrane to get.
The preparation of 2.3 reference substance solutions
Precision weighs Quercetin -3-O- gentiobioside with cape jasmine, Camellianoside, Tsubakioside A, kaempferia galamga respectively
Phenol -3-O- rutinoside, Isorhamnetin -3-O- rutinoside reference substance are appropriate, add the dissolution of 70% ethanol solution and constant volume scale,
Shake up to get mass concentration be respectively 0.0625mg/mL, 0.250mg/mL, 0.0675mg/mL, 0.0625mg/mL,
The mixed reference substance solution of 0.0500mg/mL.
2.4 methodological study
2.4.1 specificity is tested
It is molten with 70% ethyl alcohol of Extraction solvent in order to investigate the Extraction solvent of test solution and the disturbed condition of mobile phase
Liquid carries out specificity test measurement by chromatographic condition under " 2.1 " item, and result is that noiseless solvent peak goes out in the chromatogram of acquisition
It is existing, show that Extraction solvent and mobile phase are substantially noiseless.(see Fig. 1)
2.4.2 integrity test
S1 medicinal material (Guizhou Province town Ning County) powder about 1g is taken, it is accurately weighed, it is molten by legal system available test product below " 2.2 " item
Liquid is measured by chromatographic condition under " 2.1 " item.To investigate the integrality for acquiring finger-print, after recording 60min, with 30% tetrahydro
Furancarbinol solution--0.1% phosphate aqueous solution of acetonitrile (65:35:0) mobile phase ratio continues to be eluted to 120min, and result is color
Without chromatographic peak information after 60min in spectrogram, show to acquire 60min chromatogram can complete documentation Sabia parviflora Wall.ex Roxb chemical component
Information.(see Fig. 2)
2.4.3 precision test
Mixed reference substance solution is taken, by chromatographic condition continuous sample introduction six times under " 2.1 " item, records retention time and peak face
Product.With Isorhamnetin -3-O- rutinoside (No. 6) for reference, Quercetin -3-O- gentiobioside with cape jasmine (No. 1),
When the opposite reservation of Camellianoside (No. 2), Tsubakioside A (No. 3) and kaempferol-3-O-rutinoside (No. 4)
Between RSD value be respectively 0.16%, 0.16%, 0.28%, 0.083%；The RSD value of relative peak area is respectively 0.54%,
1.19%, 0.50%, 0.45%；Respectively less than 2.0%, the results showed that instrument precision is good.(being shown in Table 3, Fig. 3)
3 precision experiment result of table
2.4.4 repetitive test
6 parts of powder, every part of about 1g of S1 medicinal material (Guizhou Province town Ning County) is taken, it is accurately weighed, by legal system available below " 2.2 " item
Test sample solution is measured by chromatographic condition under " 2.1 " item, records retention time and peak area.With Isorhamnetin -3-O- rutinoside
(No. 6) are reference, Quercetin -3-O- gentiobioside with cape jasmine (No. 1), Camellianoside (No. 2), Tsubakioside A (3
Number) and kaempferol-3-O-rutinoside (No. 4) retention time RSD value be respectively 0.084%, 0086%, 0.038%,
0.079%；The RSD value of relative peak area is respectively 1.0%, 0.63%, 0.77%, 1.9%；Respectively less than 2.0%, show the party
Method repeatability is good.(being shown in Table 4, Fig. 4)
4 repetitive test result of table
2.4.5 stability test
S1 medicinal material (Guizhou Province town Ning County) powder, about 1g is taken, it is accurately weighed, it is molten by legal system available test product below " 2.2 " item
Liquid, by chromatographic condition under " 2.1 " item respectively at 0,2,4,6,8,12, measure in accordance with the law for 24 hours, record retention time and peak area.With
Isorhamnetin -3-O- rutinoside (No. 6) are reference, Quercetin -3-O- gentiobioside with cape jasmine (No. 1), Camellianoside (2
Number), the RSD value of the retention time of Tsubakioside A (No. 3) and kaempferol-3-O-rutinoside (No. 4) be respectively
0.065%, 0.077%, 0.047%, 0.030%；The RSD value of relative peak area is respectively 0.92%, 0.55%, 0.32%,
1.6%；Respectively less than 2.0%, the results showed that test solution keeps stablizing interior for 24 hours.(being shown in Table 5, Fig. 5)
5 stability test result of table
The foundation of 2.5 finger-prints and similarity evaluation
2.5.1 the foundation of finger-print
By 11 batches of Sabia parviflora Wall.ex Roxb medicinal powders respectively according to legal system available test sample solution below " 2.2 " item, according to " 2.1 "
Chromatographic condition is measured under, records the chromatography of 60min.15 shared peaks are obtained in comparison chromatogram；When recording its reservation
Between and shared peak peak area, be shown in Table 6 and table 8；Wherein 1 in test solution, 2,3,4, No. 6 peaks compare ownership with reference substance is mixed
For Quercetin -3-O- gentiobioside with cape jasmine, Camellianoside, Tsubakioside A, kaempferol-3-O-rutinoside, different
Rhamnetin -3-O- rutinoside calculates each shared fingerprint peaks using No. 6 peak Isorhamnetin -3-O- rutinosides as referring to peak
Relative retention time and peak area ratio, the results showed that, each shared fingerprint peaks relative retention time, peak area ratio are relatively steady
It is fixed, 7 and table 9 are shown in Table, the technical requirements of traditional Chinese medicine fingerprint are met.
The retention time (min) of 15 characteristic peaks of 6 11 batches of Sabia parviflora Wall.ex Roxb medicinal material leaves of table
| Serial number | F1 | F2 | F3 | F4 | F5 | F6(S) | F7 | F8 | F9 | F10 | F11 | F12 | F13 | F14 | F15 |
| S1 | 10.430 | 12.107 | 16.817 | 19.483 | 22.090 | 23.380 | 26.103 | 36.360 | 38.187 | 38.600 | 39.020 | 41.640 | 42.310 | 52.747 | 53.507 |
| S2 | 10.390 | 12.090 | 16.763 | 19.443 | 22.080 | 23.380 | 26.077 | 36.363 | 38.200 | 38.607 | 39.023 | 41.673 | 42.337 | 52.757 | 53.510 |
| S3 | 10.433 | 12.100 | 16.777 | 19.453 | 22.067 | 23.393 | 26.080 | 36.347 | 38.180 | 38.583 | 39.000 | 41.627 | 42.280 | 52.740 | 53.497 |
| S4 | 10.420 | 12.090 | 16.780 | 19.447 | 22.063 | 23.360 | 26.083 | 36.343 | 38.157 | 38.580 | 39.003 | 41.610 | 42.283 | 52.760 | 53.507 |
| S5 | 10.437 | 12.017 | 16.680 | 19.390 | 22.047 | 23.347 | 26.060 | 36.350 | 38.170 | 38.593 | 39.013 | 41.643 | 42.317 | 52.760 | 53.510 |
| S6 | 10.443 | 12.133 | 16.847 | 19.517 | 22.110 | 23.433 | 25.933 | 36.343 | 38.177 | 38.577 | 38.990 | 41.617 | 42.270 | 52.720 | 53.467 |
| S7 | 10.438 | 12.107 | 16.817 | 19.487 | 22.090 | 23.400 | 26.097 | 36.340 | 38.183 | 38.567 | 38.977 | 41.597 | 42.243 | 52.717 | 53.467 |
| S8 | 10.443 | 12.043 | 16.733 | 19.443 | 22.060 | 23.367 | 26.083 | 36.327 | 38.150 | 38.550 | 38.963 | 41.567 | 42.223 | 52.720 | 53.467 |
| S9 | 10.440 | 12.087 | 16.783 | 19.463 | 22.073 | 23.367 | 26.093 | 36.333 | 38.160 | 38.560 | 38.973 | 41.583 | 42.237 | 52.713 | 53.463 |
| S10 | 10.443 | 12.063 | 16.767 | 19.457 | 22.067 | 23.363 | 26.087 | 36.323 | 38.143 | 38.550 | 38.967 | 41.567 | 42.227 | 52.717 | 53.463 |
| S11 | 10.443 | 12.053 | 16.720 | 19.430 | 22.063 | 23.383 | 26.073 | 36.327 | 38.153 | 38.553 | 38.967 | 41.573 | 42.227 | 52.717 | 53.463 |
The relative retention time of 15 characteristic peaks of 7 11 batches of Sabia parviflora Wall.ex Roxb medicinal material leaves of table
| Serial number | F1 | F2 | F3 | F4 | F5 | F6(S) | F7 | F8 | F9 | F10 | F11 | F12 | F13 | F14 | F15 |
| S1 | 0.446 | 0.518 | 0.719 | 0.833 | 0.945 | 1.000 | 1.116 | 1.555 | 1.633 | 1.651 | 1.669 | 1.781 | 1.810 | 2.256 | 2.289 |
| S2 | 0.444 | 0.517 | 0.717 | 0.832 | 0.944 | 1.000 | 1.115 | 1.555 | 1.634 | 1.651 | 1.669 | 1.782 | 1.811 | 2.257 | 2.289 |
| S3 | 0.446 | 0.517 | 0.717 | 0.832 | 0.943 | 1.000 | 1.115 | 1.554 | 1.632 | 1.649 | 1.667 | 1.779 | 1.807 | 2.255 | 2.287 |
| S4 | 0.446 | 0.518 | 0.718 | 0.832 | 0.944 | 1.000 | 1.117 | 1.556 | 1.633 | 1.652 | 1.670 | 1.781 | 1.810 | 2.259 | 2.291 |
| S5 | 0.447 | 0.515 | 0.714 | 0.831 | 0.944 | 1.000 | 1.116 | 1.557 | 1.635 | 1.653 | 1.671 | 1.784 | 1.813 | 2.260 | 2.292 |
| S6 | 0.446 | 0.518 | 0.719 | 0.833 | 0.944 | 1.000 | 1.107 | 1.551 | 1.629 | 1.646 | 1.664 | 1.776 | 1.804 | 2.250 | 2.282 |
| S7 | 0.446 | 0.517 | 0.719 | 0.833 | 0.944 | 1.000 | 1.115 | 1.553 | 1.632 | 1.648 | 1.666 | 1.778 | 1.805 | 2.253 | 2.285 |
| S8 | 0.447 | 0.515 | 0.716 | 0.832 | 0.944 | 1.000 | 1.116 | 1.555 | 1.633 | 1.650 | 1.667 | 1.779 | 1.807 | 2.256 | 2.288 |
| S9 | 0.447 | 0.517 | 0.718 | 0.833 | 0.945 | 1.000 | 1.117 | 1.555 | 1.633 | 1.650 | 1.668 | 1.780 | 1.808 | 2.256 | 2.288 |
| S10 | 0.447 | 0.516 | 0.718 | 0.833 | 0.945 | 1.000 | 1.117 | 1.555 | 1.633 | 1.650 | 1.668 | 1.779 | 1.807 | 2.256 | 2.288 |
| S11 | 0.447 | 0.515 | 0.715 | 0.831 | 0.944 | 1.000 | 1.115 | 1.554 | 1.632 | 1.649 | 1.666 | 1.778 | 1.806 | 2.255 | 2.286 |
| Average value | 0.446 | 0.517 | 0.717 | 0.832 | 0.944 | 1.000 | 1.115 | 1.55 | 1.633 | 1.650 | 1.67 | 1.78 | 1.808 | 2.256 | 2.288 |
| RSD/% | 0.20 | 0.23 | 0.23 | 0.095 | 0.064 | 0 | 025 | 0.10 | 0.092 | 0.12 | 0.12 | 0.12 | 0.15 | 0.12 | 0.12 |
The peak area result of 15 characteristic peaks of 8 11 batches of Sabia parviflora Wall.ex Roxb medicinal material leaves of table
| Serial number | F1 | F2 | F3 | F4 | F5 | F6(S) | F7 | F8 | F9 | F10 | F11 | F12 | F13 | F14 | F15 |
| S1 | 22.6681 | 81.4019 | 33.6046 | 6.3652 | 16.2135 | 17.3574 | 3.1195 | 1.5031 | 2.4676 | 8.1478 | 1.1191 | 12.8512 | 1.4358 | 2.4492 | 4.4361 |
| S2 | 5.1379 | 14.5497 | 9.5478 | 8.4082 | 5.9568 | 4.5198 | 0.4455 | 2.2973 | 4.3179 | 15.1276 | 1.7261 | 27.9482 | 24199 | 4.5620 | 8.3865 |
| S3 | 0.7236 | 25.3992 | 12.2883 | 6.7380 | 7.9613 | 5.2783 | 1.6378 | 2.7493 | 4.5661 | 17.8988 | 1.9498 | 30.4072 | 2.4274 | 2.8144 | 4.4816 |
| S4 | 1.5256 | 33.5166 | 5.3214 | 0.8443 | 7.0014 | 2.1980 | 1.2336 | 0.3022 | 0.6011 | 2.3721 | 0.3507 | 4.6980 | 0.4896 | 6.4887 | 27.8631 |
| S5 | 1.8281 | 49.4992 | 17.6173 | 3.0260 | 4.6972 | 1.6780 | 3.0343 | 0.4453 | 0.8111 | 2.5829 | 0.3698 | 4.6500 | 0.5193 | 4.0844 | 13.1361 |
| S6 | 15.8214 | 63.7139 | 38.5395 | 9.0725 | 7.5938 | 13.8495 | 2.7954 | 2.5737 | 4.0588 | 15.3862 | 2.0155 | 23.6898 | 3.5474 | 1.0008 | 1.0774 |
| S7 | 6.2345 | 37.3923 | 11.5335 | 3.5893 | 13.8555 | 8.1630 | 2.1910 | 4.3658 | 7.3410 | 22.1462 | 3.0973 | 32.1558 | 4.3356 | 0.4330 | 0.3257 |
| S8 | 4.5015 | 62.2667 | 16.1834 | 1.6681 | 13.0942 | 7.7243 | 0.4424 | 1.7186 | 3.1482 | 10.0092 | 1.3934 | 17.3711 | 2.6274 | 1.7391 | 1.6520 |
| S9 | 9.6455 | 44.9911 | 15.3760 | 4.8478 | 8.6056 | 10.5138 | 1.5522 | 2.0313 | 3.5999 | 11.9723 | 1.6653 | 19.6869 | 2.8670 | 0.9519 | 1.3684 |
| S10 | 3.6301 | 56.2180 | 17.5943 | 8.8428 | 4.5452 | 4.0078 | 3.2934 | 0.9361 | 1.9184 | 5.1264 | 0.7412 | 9.6621 | 1.4946 | 1.5410 | 1.9348 |
| S11 | 6.5610 | 30.3622 | 6.5568 | 6.1679 | 7.4684 | 6.9428 | 1.4685 | 1.8445 | 3.1080 | 11.7335 | 1.6628 | 19.4244 | 2.7588 | 1.7175 | 2.3523 |
The peak area ratio of 15 characteristic peaks of 9 11 batches of Sabia parviflora Wall.ex Roxb medicinal material leaves of table
| Serial number | F1 | F2 | F3 | F4 | F5 | F6(S) | F7 | F8 | F9 | F10 | F11 | F12 | F13 | F14 | F15 |
| S1 | 1.305 | 4.690 | 1.936 | 0.367 | 0.934 | 1.000 | 0.180 | 0.087 | 0.142 | 0.469 | 0.064 | 0.740 | 0.083 | 0.141 | 0.256 |
| S2 | 1.137 | 3.219 | 2.112 | 1.860 | 1.318 | 1.000 | 0.099 | 0.508 | 0.955 | 3.347 | 0.382 | 6.184 | 0.535 | 1.009 | 1.856 |
| S3 | 0.137 | 4.812 | 2.328 | 1.277 | 1.508 | 1.000 | 0.310 | 0.521 | 0.865 | 3.391 | 0.369 | 5.761 | 0.460 | 0.533 | 0.849 |
| S4 | 0.740 | 15.249 | 2.421 | 0.384 | 3.185 | 1.000 | 0.561 | 0.137 | 0.273 | 1.079 | 0.160 | 2.137 | 0.223 | 2.952 | 12.677 |
| \S5 | 1.089 | 29.499 | 10.499 | 1.803 | 2.799 | 1.000 | 1.808 | 0.265 | 0.483 | 1.539 | 0.220 | 2.771 | 0.309 | 2.434 | 7.828 |
| S6 | 1.142 | 4.600 | 2.783 | 0.655 | 0.548 | 1.000 | 0.202 | 0.186 | 0.293 | 1.111 | 0.146 | 1.711 | 0.256 | 0.072 | 0.078 |
| S7 | 0.764 | 4.581 | 1.413 | 0.440 | 1.697 | 1.000 | 0.268 | 0.535 | 0.899 | 2.713 | 0.379 | 3.939 | 0.531 | 0.053 | 0.040 |
| S8 | 0.583 | 8.061 | 2.095 | 0.216 | 1.695 | 1.000 | 0.057 | 0.222 | 0.408 | 1.296 | 0.180 | 2.249 | 0.340 | 0.225 | 0.214 |
| S9 | 0.917 | 4.279 | 1.462 | 0.461 | 0.819 | 1.000 | 0.148 | 0.193 | 0.342 | 1.139 | 0.158 | 1.872 | 0.273 | 0.091 | 0.130 |
| S10 | 0.906 | 14.027 | 4.390 | 2.206 | 1.134 | 1.000 | 0.822 | 0.234 | 0.479 | 1.279 | 0.185 | 2.411 | 0.373 | 0.385 | 0.483 |
| S11 | 0.945 | 4.373 | 0.944 | 0.888 | 1.076 | 1.000 | 0.212 | 0.266 | 0.448 | 1.690 | 0.239 | 2.799 | 0.397 | 0.247 | 0.339 |
| Average value | 0.879 | 8.854 | 2.944 | 0.960 | 1.519 | 1.003 | 0.424 | 0.287 | 0.508 | 1.858 | 0.226 | 2.961 | 0.344 | 0.740 | 2.25 |
| RSD/% | 36.7 | 90.2 | 90.1 | 73.9 | 53.6 | 0 | 120.2 | 55.7 | 54.2 | 49.9 | 47.3 | 56.9 | 39.6 | 136.5 | 183.8 |
2.5.2 similarity evaluation result
The HPLC map of 11 batches of Sabia parviflora Wall.ex Roxb medicinal materials is imported into finger-print software (2004A editions), sets S1 as reference
Spectrum, using Supplements, time window width 0.5, control map generation method is median method, establishes finger-print and sees Fig. 6,
The shared peak control map generated is shown in that Fig. 7, the uv absorption spectra of 5 characteristic components are shown in 8.Similarity calculation evaluation result table
Bright, the fingerprint similarity calculated result of each place of production Sabia parviflora Wall.ex Roxb medicinal material is other than S9, S10 and S11, the finger of other batches
Line map similarity illustrates that the Sabia parviflora Wall.ex Roxb medicinal material chemical component of different sources is relatively more consistent, as a result sees 0.80 or more
Table 10.
10 similarity evaluation result of table
2.6 Stoichiometric analysis
Only it is difficult to react the similarities and differences for reflecting different batches of sample rooms comprehensively from similarity difference.Therefore further use SPSS
16.0 softwares carry out clustering (HCA) and principal component to the shared peak data of different batches Sabia parviflora Wall.ex Roxb medicinal materials fingerprint
It analyzes (PCA).
2.6.1 clustering (HCA)
Using 16.0 statistical analysis software of SPSS, using in hierarchical clustering method group distance method, vector COS distance as
Sample is estimated, and carries out clustering to each peak area standardized data of 11 batch Sabia parviflora Wall.ex Roxb medicinal materials, and draw dendrogram,
See Fig. 9.When criterion distance is 20, three categories are roughly divided into, I class includes S4, S5, S10；II class includes S1, S6；III class
Including S2, S3, S7, S8, S9, S11.When criterion distance is 5, nine major class can be divided into: Change at Luoping County in Yunnan Province (S10), expensive
Town Ning County, state province (S1), Xingyi City, Guizhou Province (S11), Guizhou Province Anlong County (S7), Guangxi province Xilin County (S9), Yunnan Province master of great learning and integrity
The sample in county (S8) individually gathers for one kind, and it is one that Guangxi province Tianlin County (S2) and Guizhou university of TCM, which introduce a fine variety (S3) number sample to gather,
Class, it is seen that cloud, expensive, Guang San save the influence due to multiple environmental factors such as topography-geomorphology, height above sea level weathers, lead to medicinal material intrinsic chemical
Component content is distinct；Individually gather the neighbour for one kind, S4 and S5 for Guizhou Province Ceheng County in Guizhou Province, the town Po Mei, Ceheng County (S6)
Gather for one kind in town, it is seen that the even same place of production also there are individual batch quality of medicinal material to have differences；Phase between each batch sample
Guan Xingyu similarity analysis result is more consistent.
2.6.2 principal component analysis (PCA)
In order to more directly evaluate 15 shared ingredients to the resolution capability of sample, with the characteristic root and contribution rate of principal component
The alternatively foundation of principal component carries out PCA analysis to 11 batches of Sabia parviflora Wall.ex Roxb medicinal material samples using SPSS16.0 editions softwares, asks
The characteristic value and its variance of correlation matrix out, is shown in Table 11.It is extraction standard with characteristic value > 1, obtains the accumulative side of preceding 3 factors
Poor contribution rate is 87.375%.PCA rubble figure is shown in Figure 10, and the gradient for extract 3 factors that take the lead in is more precipitous and subsequent
The gradient of formation is more gentle, therefore selects this 3 factors for main component 1,2,3.Principal component loading matrix reflects each variable
To the contribution and action direction of principal component.In addition to sharing peak F7、F14、F15Principal component 1 is negatively correlated, remaining equal positive
It closes, wherein with F8~F13Contribution it is maximum；Shared peak F1~F7Principal component 2 is positively correlated, peak F is shared8~F15To principal component 2
It is negatively correlated, wherein F1~F3、F6And F7Maximum is contributed to principal component 2；Except F3、F4、F7、F10And F12Principal component 3 is negatively correlated,
Remaining is positively correlated, F5It is maximum to the contribution of principal component 3, it is shown in Table 12.
11 characteristic value of table and variance contribution ratio
12 principal component loading matrix of table
Above-mentioned principal component load value is calculated, obtains the linear model of each principal component: where Z1、Z2、Z3Table respectively
Show the 1st, 2,3 principal component, Z represents the synthesis principal component for combining 3 principal components to obtain, X1~X15Respectively indicate 15 shared peaks
The standardized data of peak area.After each sample data is substituted into above-mentioned model, the principal component scores of each batch sample are obtained, are shown in Table
13；The comprehensive score highest of S1, best in quality, followed by S6 and No. S7 batch of sample；And with the 1st of sample the, 2,3 principal component scores
Three-dimensional scatter plot is done, sees that Figure 11, the classification results and HCA result of 11 batches of samples are more consistent.
Z1=0.404X1+0.290X2+0.284X3+0.394X4+0.506X5+0.596X6-0.030X7+0.938X8+
0.926X9+0.920X10+0.949X11+0.876X12+0.942X13-0.779X14-0.80X15；
Z2=0.798X1+0.940X2+0.867X3+0.220X4+0.349X5+0.706X6+0.690X7-0.275X8-
0.323X9-0.346X10-0.277X11-0.415X12-0.186X13-0.298X14-0.231X15；
Z3=0.135X1+0.183X2-0.140X3-0.791X4+0.740X5+0.216X6-0.412X7+0.054X8+
0.047X9-0.017X10+0.054X11-0.069X12+0.110X13+0.138X14+0.244X15；
Z=1.337X1+1.413X2+1.011X3-0.177X4+1.595X5+1.518X6+0.248X7+0.717X8+
0.650X9+0.557X10+0.726X11+0.329X12+0.866X13-0.939X14-0.787X15
13 sample principal component scores of table
3 conclusions
This experiment uses diode array detector, has investigated the detection wave of 220nm, 254nm, 270nm, 360nm respectively
It is long, the results showed that it can preferably reflect the UV absorption of each ingredient under 360nm wavelength, Chromatographic information is abundant and baseline is steady, because
This selection 360nm；To chromatographic column Phenomenex Synergi Hydro-RP 80A (250 × 4.6mm, 5 μm),
Phenomenex Kinetex-C18(100 × 4.6mm, 2.6 μm), Thermo Accucore-C18(150 × 4.6mm, 2.6 μ
M), Thermo Hyperil (250 × 4.6mm, 5 μm) carries out analysis comparison, and measurement result shows Thermo Accucore-C18
(150 × 4.6mm, 2.6 μm) chromatographic column is more compared with other three kinds of chromatographic column appearances, and separating degree is preferable, therefore the column is selected to carry out
Fingerprint map analyzing；Respectively to methanol-water, -0.1% phosphoric acid water of methanol, acetonitrile-water, methanol-acetonitrile-water, first in mobile phase
- 0.1% glacial acetic acid water of alcohol, -0.1% phosphoric acid water of methanol-acetonitrile, -0.1% formic acid water of methanol-acetonitrile, tetrahydrofuran-water, 5%
Tetrahydrofurfuryl carbinol solution--0.1% phosphate aqueous solution of acetonitrile, methanol -0.1% phosphoric acid of -5% tetrahydrofuran acetonitrile solution are water-soluble
Liquid, 10% tetrahydrofurfuryl carbinol solution--0.1% phosphate aqueous solution of acetonitrile, 20% tetrahydrofurfuryl carbinol solution-acetonitrile -0.1%
Phosphate aqueous solution, 30% tetrahydrofurfuryl carbinol solution--0.1% phosphate aqueous solution of acetonitrile, 40% tetrahydrofurfuryl carbinol solution-second
14 kinds of flow phase system gradient elution separation situations such as -0.1% phosphate aqueous solution of nitrile carry out test comparison, the results showed that use
Chromatographic peak separating effect is best when 30% tetrahydrofurfuryl carbinol solution--0.1% phosphate aqueous solution of acetonitrile is mobile phase, most of
Chromatographic peak reaches baseline separation, and each chromatographic peak purity is higher；It is 25 DEG C, 30 DEG C and 35 DEG C that column temperature, which is respectively set, compares its point
From effect, the results showed that the symmetry of separating effect and chromatographic peak is preferable when column temperature is 30 DEG C, therefore selects 30 DEG C.This experiment is to mentioning
Take method (ultrasound, reflux, cold soaking), Extraction solvent (methanol, ethyl alcohol), the ratio of Extraction solvent (50%, 60%, 70%,
80%, 90%), solid-liquid ratio (1:10,1:15,1:20,1:25,1:30) is investigated, and to sum up determines " 2.2 " item test solution
Preparation.
The present invention establishes the Sabia parviflora Wall.ex Roxb medicinal materials fingerprint discrimination method of 5 flavonoids, can relatively comprehensively
Ground reflects the interior quality of the medicinal material.By successively using similarity analysis, clustering to 15 obtained shared chromatographic peaks
More fully analyzed with 3 kinds of methods of principal component analysis, as the result is shown the shared peak relative retention time difference of sample room compared with
It is small, but there is some difference for peak area, shows that chemical component contained by different sources Sabia parviflora Wall.ex Roxb medicinal material is more consistent；This hair
The bright quality evaluation for Sabia parviflora Wall.ex Roxb medicinal material establishes a set of more perfect scientific system, can be used as Sabia parviflora Wall.ex Roxb medicinal material
The scientific basis of base chiller and quality control.
Experiments have shown that, the method for the foundation is reliable and stable, and finger-print is relatively stable above, and the present invention is clear to improve little Hua
What quality evaluation system, medicine elementary source identification and the quality of wind rattan medicinal material controlled provides scientific basis.
Compared with prior art, this method has easy, stable, precision height, high repeatability and other advantages；Also with this method
It more can comprehensively reflect the type and quantity of contained chemical component in Sabia parviflora Wall.ex Roxb, and then whole description is carried out to its quality
And evaluation.And the Sabia parviflora Wall.ex Roxb finger-print chemical component that is detected with this method is relatively more, each characteristic peak height ratio
Moderate, baseline is more steady, and separating degree and peak shape are good, and column effect is high.
Detailed description of the invention
Fig. 1 is specificity test HPLC chromatogram stacking chart；Wherein, A-70% ethanol solution；B- mixed reference substance solution；C-
Test solution；
Fig. 2 is integrity test HPLC chromatogram stacking chart；
Fig. 3 is precision test HPLC chromatogram stacking chart；
Fig. 4 is repetitive test HPLC chromatogram stacking chart；
Fig. 5 is stability test HPLC chromatogram stacking chart；
Fig. 6 is 11 batches of Sabia parviflora Wall.ex Roxb medicinal material HPLC common pattern stacking charts (time window width 0.5, median method)；
Fig. 7 is Sabia parviflora Wall.ex Roxb medicinal material HPLC reference fingerprint；I-mixing reference substance map；II-shared peak control refers to
Line map；1- Quercetin -3-O- gentiobioside with cape jasmine；2-Camellianoside；3-Tsubakioside A；4- Kaempferol -3-
O- rutinoside；6- Isorhamnetin -3-O- rutinoside；
Fig. 8 is test sample and the uv absorption spectra for mixing contrast solution；
Fig. 9 is 11 batches of Sabia parviflora Wall.ex Roxb medicinal material clustering dendrograms；
Figure 10 is principal component rubble figure；
Figure 11 is 11 batches of Sabia parviflora Wall.ex Roxb medicinal material principal component scores figures.
Below with reference to embodiment, the present invention is further illustrated.
Specific embodiment
Embodiment:
A kind of HPLC fingerprint of Sabia parviflora Wall.ex Roxb, comprising the following steps:
(1) preparation of mixed reference substance solution: respectively precision weigh Quercetin -3-O- gentiobioside with cape jasmine,
Camellianoside, Tsubakioside A, kaempferol-3-O-rutinoside, the control of Isorhamnetin -3-O- rutinoside
Product, add 70% ethanol solution dissolve, shake up, be made Quercetin -3-O- gentiobioside with cape jasmine mass concentration be 0.0625mg/mL,
Camellianoside mass concentration is 0.250mg/mL, Tsubakioside A mass concentration is 0.0675mg/mL, kaempferia galamga
Phenol -3-O- rutinoside mass concentration is 0.0625mg/mL, Isorhamnetin -3-O- rutinoside mass concentration is 0.0500mg/
The mixed reference substance solution of mL；
(2) preparation of test solution: accurately weighed Sabia parviflora Wall.ex Roxb powder 1g is set in 50mL stuffed conical flask, accurate
Adding 70% ethanol solution 15mL, weighed weight is 100W in power, and frequency is ultrasonic extraction 60min under the conditions of 80Hz, it lets cool,
With 70% ethanol solution mend weight, shake up, filter, filtrate with 0.45 μm of organic filtering with microporous membrane to get；
(3) chromatographic condition that finger-print is established: chromatographic column: Thermo Accucore-C18, 150 × 4.6mm, 2.6 μm；
Mobile phase: 30% tetrahydrofurfuryl carbinol solution is A phase, and acetonitrile is B phase, and 0.1% phosphate aqueous solution is C phase；Gradient elution, detection
Wavelength is 360nm, flow velocity 1mL/min, 30 DEG C of column temperature, 10 μ L of sample volume；Record spectrogram obtains Sabia parviflora Wall.ex Roxb medicinal material
HPLC finger-print；Gradient elution program: 0-5min:A (5% → 12%) and B (3% → 6%)；5-15min:A (12% →
And B (6% → 8%) 10%)；15-20min:A (10% → 20%) and B (8% → 10%)；20-35min:A (20% →
And B (10% → 28%) 53%)；35-45min:A (53%) and B (28%)；45-50min:A (53% → 70%) and B (28%
→ 30%)；50-60min:A (70% → 65%) and B (30% → 35%).
In 15 shared peaks, No. 1 peak is Quercetin -3-O- gentiobioside with cape jasmine, and No. 2 peaks are Camellianoside, 3
Number peak is Tsubakioside A, and No. 4 peaks are kaempferol-3-O-rutinoside, and No. 6 peaks are Isorhamnetin -3-O- rutinoside；
15 shared peaks are referring to peak, relative retention time point with No. 6 peak Isorhamnetin -3-O- rutinosides
It Wei not 0.444-0.447,0.515-0.518,0.714-0.719,0.831-0.833,0.943-0.945,1.000,1.107-
1.117、1.551-1.557、1.629-1.635、1.646-1.653、1.664-1.671、1.776-1.784、1.804-
1.813、2.250-2.260、2.282-2.292。
Claims (6)
1. a kind of HPLC fingerprint of Sabia parviflora Wall.ex Roxb, it is characterised in that: the following steps are included:
(1) preparation of mixed reference substance solution: respectively precision weigh Quercetin -3-O- gentiobioside with cape jasmine, Camellianoside,
Tsubakioside A, kaempferol-3-O-rutinoside, Isorhamnetin -3-O- rutinoside reference substance, add 70% ethanol solution
Dissolution, shakes up, and it is that 0.0625mg/mL, Camellianoside mass are dense that Quercetin -3-O- gentiobioside with cape jasmine mass concentration, which is made,
Degree is 0.250mg/mL, Tsubakioside A mass concentration is 0.0675mg/mL, kaempferol-3-O-rutinoside quality is dense
Degree be 0.0625mg/mL, the mixed reference substance solution that Isorhamnetin -3-O- rutinoside mass concentration is 0.0500mg/mL；
(2) preparation of test solution: accurately weighed Sabia parviflora Wall.ex Roxb powder, precision plus the dissolution of 70% ethanol solution, it is weighed heavy
Amount, ultrasonic extraction are let cool, and are mended weight with 70% ethanol solution, are shaken up, filter, 0.45 μm of organic filtering with microporous membrane of filtrate, i.e.,
?；
(3) chromatographic condition that finger-print is established: chromatographic column: ThermoAccucore-C18, 150 × 4.6mm, 2.6 μm；Flowing
Phase: 30% tetrahydrofurfuryl carbinol solution is A phase, and acetonitrile is B phase, and 0.1% phosphate aqueous solution is C phase；Gradient elution, Detection wavelength
For 360nm, flow velocity 1mL/min, 30 DEG C of column temperature, 10 μ L of sample volume；The HPLC that record spectrogram obtains Sabia parviflora Wall.ex Roxb medicinal material refers to
Line map；
(4) according to the method for above-mentioned offer, its HPLC fingerprint the confirmation of standard fingerprint spectrogram: is established to multiple batches of Sabia parviflora Wall.ex Roxb
Map is compared by analysis and 15 shared peaks has been determined, these shared peaks constitute the fingerprint characteristic of Sabia parviflora Wall.ex Roxb, is established
Common pattern, the standard finger-print as Sabia parviflora Wall.ex Roxb medicinal material.
2. the HPLC fingerprint of Sabia parviflora Wall.ex Roxb as described in claim 1, it is characterised in that: the test sample
Solution is prepared: accurately weighed Sabia parviflora Wall.ex Roxb powder 1g is set in 50mL stuffed conical flask, precision plus 70% ethanol solution
15mL, weighed weight, ultrasonic extraction 60min are let cool, and are mended weight with 70% ethanol solution, are shaken up, filter, filtrate has with 0.45 μm
Machine filtering with microporous membrane to get.
3. the HPLC fingerprint of Sabia parviflora Wall.ex Roxb as claimed in claim 1 or 2, it is characterised in that: ultrasound mentions
When taking, power 100W, frequency 80Hz.
4. the HPLC fingerprint of Sabia parviflora Wall.ex Roxb as described in claim 1, it is characterised in that: gradient elution
When, gradient elution program is: the B of the A of 0-5min:5% → 12% and 3% → 6%；The A of 5-15min:12% → 10% and 6%
→ 8% B；The B of the A of 15-20min:10% → 20% and 8% → 10%；The A of 20-35min:20% → 53% and 10% →
28% B；The B of the A of 35-45min:53% and 28%；The B of the A of 45-50min:53% → 70% and 28% → 30%；50-
The B of the A of 60min:70% → 65% and 30% → 35%.
5. the HPLC fingerprint of Sabia parviflora Wall.ex Roxb as described in claim 1, it is characterised in that: described 15 altogether
Have in peak, No. 1 peak is Quercetin -3-O- gentiobioside with cape jasmine, and No. 2 peaks are Camellianoside, and No. 3 peaks are
TsubakiosideA, No. 4 peaks are kaempferol-3-O-rutinoside, and No. 6 peaks are Isorhamnetin -3-O- rutinoside.
6. the HPLC fingerprint of Sabia parviflora Wall.ex Roxb as described in claim 1, it is characterised in that: described 15 altogether
Have peak, with No. 6 peak Isorhamnetin -3-O- rutinosides be referring to peak, relative retention time be respectively 0.444-0.447,
0.515-0.518、0.714-0.719、0.831-0.833、0.943-0.945、1.000、1.107-1.117、1.551-
1.557、1.629-1.635、1.646-1.653、1.664-1.671、1.776-1.784、1.804-1.813、2.250-
2.260、2.282-2.292。
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