CN105911186A - Measurement method of honeysuckle and radix scutellariae granule fingerprint spectrum - Google Patents
Measurement method of honeysuckle and radix scutellariae granule fingerprint spectrum Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to a quality control method for honeysuckle and radix scutellariae granules, particularly relates to a measurement method of a honeysuckle and radix scutellariae granule fingerprint spectrum, and belongs to the technical field of medicine analysis. The method includes the steps of: 1) preparing a reference substance solution; 2) preparing an internal standard solution; 3) preparing a sample solution; and 4) performing analysis and measurement with high performance liquid chromatography-mass spectrum. Through the HPLC-MS method, chemical components of a common peak of the honeysuckle and radix scutellariae granules are accurately measured. The method is simple and accurate, has high sensitivity and good repeatability, can monitor qualities of raw material medicines, semi-products and finish products more comprehensively, and can also monitor stability of a production process.
Description
Technical field
The present invention relates to pharmaceutical analysis technical field, particularly to the assay method of a kind of Yinhuang Particle finger printing.
Background technology
The compound preparation that Yinhuang Particle system is made up of Flos Lonicerae extract, Radix Scutellariae extract, has heat-clearing and toxic substances removing, antiinflammatory etc.
Effect, is widely used in treating upper respiratory tract infection, acute tonsillitis, pharyngitis, mumps, ophthalmic diseases, burn
The diseases such as infection.At present this kind has 102 enterprises, factory what State Food and Drug Administration got the Green Light code
Family is numerous, and the difference of the aspect such as crude drug, production technology all can affect product quality in addition.
Chinese medicine fingerprint uses analysis means technology such as () spectrum, wave spectrum, chromatographs of various advanced persons to indicate Chinese medicinal components
The characteristic of colony, is to realize differentiating Chinese medicine verity, evaluation quality concordance and the Feasible Mode of product stability, has information
The features such as amount is big, characteristic strong, globality and ambiguity.Finger printing includes principal component and the analysis of non-principal component,
The chemical composition information (being embodied in relative retention time and relative peak area) of reflection has high degree of specificity and selectivity,
Can more fully hereinafter reflect the integral status of various chemical composition amounts distribution in Chinese medicine COMPLEX MIXED system, especially in present stage
In the case of the effective ingredient overwhelming majority is the clearest and the most definite, it is possible to combine various chromatograph, spectrum, wave spectrum means, identify characteristically
The true and false of Chinese medicine, with good and bad, becomes " the chemistry bar code " of Chinese medicine self.
" the HPLC characteristic spectrum of Yinhuang Particle is analyzed " paper of " pharmaceutical analysis magazine " the 8th phase of volume 29 in 2009
In, establishing Yinhuang Particle RP-HPLC finger print measuring method, flowing is acetonitrile-0.1% phosphoric acid solution mutually, gradient elution,
Flow velocity is 1.0mL/min, and the detection time is 35min, uses self ingredient chlorogenic acid peak for reference to peak, determines 12 altogether altogether
There is the peak mathematical expression as this Variety fingerprinting.One " the ultra high efficiency liquid of " assay office " the 7th phase of volume 34 in 2015
Phase chromatograph-quadrupole rod time-of-flight mass spectrometry (TOFMS) measures chemical combination composition and main component in Yinhuang Particle " in paper, establish superelevation
Effect liquid phase chromatogram-quadrupole rod flight time mass spectrum (UHPLC-QTOF-MS) measure the qualitative of active component in Yinhuang Particle and
Quantitative analysis method, with 0.5% aqueous formic acid-acetonitrile for flowing phase, gradient elution, flow velocity 0.4 mL/min, detects the time 25
In chromatogram 12 kinds principal component have been carried out detection by quantitative by min.
But, the most simple chemical information reflecting Chinese medicine of finger printing, with pharmacodynamics index onrelevant, it is difficult in accurate evaluation
Medicine product quality, and drug effect is to evaluate the ultimate index of drug quality.
Summary of the invention
For solving the problems referred to above, the present invention provides the assay method of a kind of Yinhuang Particle finger printing, uses liquid chromatograph
The method being used in conjunction with mass spectrum, accurately measures Yinhuang Particle and has the chemical composition at peak, easy to be accurate, highly sensitive, reproducible.
The present invention is achieved by the following technical solutions:
The assay method of a kind of Yinhuang Particle finger printing, it is characterised in that comprise the following steps:
(1) preparation of reference substance solution: precision weighs isorhamnetin, baicalin, baicalin, luteoloside, 4-dicaffeoylquinic acid, fresh green
Ortho acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, oroxylin, chrysin, wogonoside, wogonin, add first respectively
Alcohol dissolves, and adds isopyknic water, is respectively prepared 0.1mg/ml reference substance solution；
(2) preparation of inner mark solution: precision weighs isorhamnetin, adds methanol and dissolves, add isopyknic water, and constant volume becomes concentration
It is 30 g mL-1Inner mark solution；
(3) need testing solution preparation method: take Yinhuang Particle, add methanol solution making concentration is 40mg mL-1Sample is molten
Liquid；By sample solution and 30 g mL-1Inner mark solution equal-volume mixing, through 0.22 m microporous filter membrane filter, take subsequent filtrate make
For need testing solution；
(4) measure: utilize HPLC MS to be analyzed measuring.
Further, in described step (3), the preparation method of need testing solution is: take Yinhuang Particle, and precision weighs fine powder
1.0g, is placed in 50 mL round-bottomed flasks, and the accurate volume fraction that adds is 50% methanol aqueous solution 25mL, weighs, is heated to reflux
20min, lets cool, and mends weight, filters, obtains subsequent filtrate 1；Take subsequent filtrate 1 to mix with inner mark solution equal-volume, through 0.22 m microporous filter membrane
Filter, obtain subsequent filtrate 2 as need testing solution.
Further, described High Performance Liquid Chromatography condition is: Agela Venusil MP C18Chromatographic column (4.6mm
× 250mm, 5 m)；Condition is: column temperature 30 DEG C, flow velocity 1.0 mL min-1, detecting wavelength 235nm, sample size is: 10 μ L, with
Acetonitrile is mobile phase A, volume fraction be 0.2% phosphate aqueous solution be Mobile phase B, volume fraction is that the phosphate aqueous solution of 0.5% is
Flowing phase C carries out gradient elution.
Further, the condition of gradient elution is:
0-10 min, 5-9% mobile phase A, 95-91% Mobile phase B；10-31 min, 9-16% mobile phase A, 91-84% Mobile phase B；
31-42 min, 16% mobile phase A, 84% Mobile phase B；42-65 min, 16-20% mobile phase A, 84-80% Mobile phase B；65-
90min, 20-22% mobile phase A, 80-78% Mobile phase B；90-120min, 22% mobile phase A, 78% flowing phase C；120-150min,
22-25% mobile phase A, 78-75% flows phase C；150-170min, 25-32% mobile phase A, 75-68% flows phase C；170-
185min, 32-45% mobile phase A, 68-55% flows phase C；185-200 min, 45-60% mobile phase A, 55-40% flows phase C；
200-220 min, 60-80% mobile phase A, 40-20% flows phase C；220-250min, 80-100% mobile phase A, 20-0% flows phase
C.Described percentage ratio is percent by volume.
Further, the condition of described mass spectrography is: use ESI ion source, negative ions alternative scanning mode；Ion trap
Mass analyzer, mass scan range: 50～1500 m/z；Scanning speed 26000 m/z s-1；Spray pressure power 35.0psi；
It is dried temperature 350 DEG C；Dry gas stream speed 9L min-1；Capillary voltage 4000 V；Collision gas: helium.
Beneficial effects of the present invention:
(1) during gradient elution, have selected different time sections and select different acid concentration (phosphoric acid of 0.2% and 0.5%) to enter
Row eluting, is flowed phosphoric acid concentration in mutually by change, and good separating effect preferably differentiates the chemical composition at total peak.
(2) the present invention is directed to construction features and the physicochemical characteristics of effective ingredient contained by finished product, to need testing solution preparation side
The conditions such as method, flowing phase, elution program, chromatographic column and mass spectrometry parameters are screened and have been optimized, beneficially liquid chromatograph and mass spectrum
Be used in conjunction, and method repeatability and good stability；20 the total peaks chosen all have been carried out linear relationship investigation, and sample size exists
In the range of being equivalent to sample 0.1mg-0.5mg, each total crest line sexual relationship is good.
(3) selecting isorhamnetin is object of reference, and the test liquid containing internal standard material carries out the mensuration of finger printing, uses
The relative peak area ratio at total peak and internal standard peak is as the mathematical expression of this finger printing, so than generally selection Chinese medicine self
Composition does with reference to the relative peak area calculating each total peak, more can embody the absolute change of each total peak content and relative change.
(4) the method can more fully monitor raw medicinal material, semi-finished product and end product quality, stablizing of monitoring production technology
Property.
Accompanying drawing explanation
Fig. 1 is the Yinhuang Particle finger printing that embodiment 1 obtains.
Fig. 2 is that the present invention has carried out determining fingerprint pattern to 100 batches of Yinhuang Particles, uses median method to generate comparison fingerprint
Collection of illustrative plates.
Detailed description of the invention
Below by embodiment, the present invention will be further elaborated, and the description below is only for explaining the present invention, not
Its content is defined.
1.1 instrument
Waters e2695 high performance liquid chromatograph (Waters, US), the Waters 2998 UV-detector (U.S.
Waters company), Waters Empower chromatographic work station (Waters, US)；AGBP210S electronic balance
(Sartorius company)；MILLIPORE water purification machine (MILLIPORE company)；Agela Venusil MP C18Chromatographic column
(4.6mm × 250mm, 5 m) (Tianjin Bonaaijieer Technology Co., Ltd).
1.2 reagent
Isorhamnetin (lot number: 110860-200406), baicalin (lot number: 110715-200514), baicalin (lot number:
111595-200301), luteoloside (lot number: 111720-200603) is purchased from National Institute for Food and Drugs Control.Hidden green former
Acid (lot number: 14030213), neochlorogenic acid (lot number: 13112712), 3,5-Dicaffeoylquinic acid (lot number: 14041309), different green former
Acid B (lot number: 14022812), 4,5-Dicaffeoylquinic acid (lot number: 14022805), oroxylin (lot number: 14062410), chrysin
(lot number: 13080712), wogonoside (lot number: 13120401), wogonin (lot number: 13101809) purchased from Chengdu general
Rui Fa Science and Technology Development Co., Ltd., purity > 98%.Phase chromatography-use acetonitrile is chromatographically pure, and other reagent are analytical pure, test
It is purchased from pharmacy with Yinhuang Particle sample, derives from 100 batch samples of 36 different manufacturers.
Embodiment 1
A kind of Yinhuang Particle finger print measuring method, it is characterised in that comprise the following steps:
(1) preparation of reference substance solution: precision weighs baicalin, baicalin, luteoloside, 4-dicaffeoylquinic acid, neochlorogenic acid, different green
Ortho acid A, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, oroxylin, chrysin, wogonoside, wogonin, add methanol respectively and dissolve, then
Add isopyknic water, be respectively prepared the reference substance solution of 0.1mg/ml, keep in Dark Place at 4 DEG C.
(2) preparation of inner mark solution: precision weighs isorhamnetin, adds methanol and dissolves, add isopyknic water, and constant volume becomes
Concentration is 30 g mL-1Inner mark solution.
The selection of internal standard substance:
The comparisons such as paeonol, salvianolic acid B, puerarin, isorhamnetin, Hesperidin, kaempferol, Quercetin, Quercitroside are investigated altogether
It is internal standard that product have finally chosen isorhamnetin.The retention time of isorhamnetin is about 196 min, reaches baseline with adjacent peak and divides
From, noiseless, the separating degree of adjacent peak is equal > 1.5.
The selection of internal standard substance solvent:
Internal standard substance first dissolves with methanol, adds isopyknic aqueous solution, is prepared as internal standard substance solution.Internal standard substance solution is through ultrasonic
(20min) clarify after, mix with test liquid the most again, still clarify after mixing, and the most muddy in placement 24h.Therefore join by the method
Inner mark solution processed.
The determination of internal standard substance concentration:
Randomly select 10 Yinhuang Particle samples, prepare sample solution, and add the inner mark solution of equal-volume variable concentrations, mixed
Even, enter high performance liquid chromatograph and measure, select the isorhamnetin concentration that in spectrogram, peak area is moderate, to determine the dense of internal standard substance
Degree.Through investigating, determine that the concentration of isorhamnetin is 30 g mL-1。
(3) need testing solution preparation method: take Yinhuang Particle finely ground, precision weighs fine powder 1.0g, is placed in 50 mL round bottoms and burns
In bottle, the accurate volume fraction that adds is 50% methanol aqueous solution 25mL, weighs, is heated to reflux 20min, let cool, mend weight, filters,
Subsequent filtrate 1；Take subsequent filtrate 1 to mix with inner mark solution equal-volume, filter through 0.22 m microporous filter membrane, obtain subsequent filtrate 2 as examination
Product solution；
(4) measure: HPLC MS measures.
High Performance Liquid Chromatography condition is: Agela Venusil MP C18(4.6mm × 250mm, 5 m) for chromatographic column；
Condition is: column temperature 30 DEG C, flow velocity 1.0mL min-1, detects wavelength 235nm, and sample size is 10 μ L, with acetonitrile as mobile phase A,
Volume fraction be 0.2% phosphate aqueous solution be Mobile phase B, volume fraction be 0.5% phosphate aqueous solution for flowing phase C carry out gradient
Eluting.
The condition of gradient elution is shown in Table 1:
Described percentage ratio is percent by volume.
(5) chromatogram obtained according to the method described above, as shown in Figure 1.
With isorhamnetin as reference, having demarcated 20 total peaks, total peak area accounts for more than the 85% of the gross area, measures 12
The reference substance solution of individual composition, by the comparison with reference substance retention time and ultra-violet absorption spectrum, it is determined that wherein 1,3,4,
7,8,9,11,16,17,18,19, No. 20 chromatographic peaks are respectively neochlorogenic acid, chlorogenic acid, 4-dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, different green
Ortho acid A, 4,5-Dicaffeoylquinic acid, baicalin, wogonoside, baicalin, wogonin, chrysin, oroxylin.
In conjunction with interpretation of mass spectra and the comparison of reference substance, determining the chemical composition at 14 total peaks altogether, analysis result is shown in
Table 2.The condition of mass spectrography is: use ESI ion source, negative ions alternative scanning mode；Ion strap mass analyzer, quality is swept
Retouch scope: 50～1500 m/z；Scanning speed 26000 m/z s-1；Spray pressure power 35.0psi；It is dried temperature 350 DEG C；
Dry gas stream speed 9L min-1；Capillary voltage 4000 V；Collision gas: helium.
Table 2 is part total peak component resolving in Yinhuang Particle.
The investigation of 2.1 linear relationships
Accurately weigh 2.5g Yinhuang Particle, accurate add 50% methanol solution 25mL, prepare test liquid, draw respectively 1mL, 2mL,
3mL, 4mL, 5mL test liquid, in 5mL measuring bottle, adds 50% methanol constant volume to scale, shakes up, and equal-volume adds variable concentrations
Isorhamnetin inner mark solution, preparing altogether containing sample concentration is 0.01g mL-1、0.02 g·mL -1、0.03 g·mL -1、
0.04 g·mL -1、0.05 g·mL -1Test liquid, make the concentration of contained internal standard material be respectively 10 g mL-1、20µ
g·mL -1、30µg·mL -1、40µg·mL -1、50µg·mL -1.Sample introduction 10 L respectively, is measured by chromatographic condition sample introduction, with
Concentration X (g mL-1) is abscissa, carries out linear regression with each peak and internal standard peak area ratio Y vertical coordinate, and result shows
Sample size is in suitable sample 100 ~ 500 g range, and 20 total peak component linear relations are good, and internal standard material is at sample size
0.1 ~ 0.5 g range internal linear relation is good.Linear relationship is shown in Table 3.
2.2 precision test
Take same sample test liquid, 10 μ L sample introductions, continuous sample introduction 5 times, measure by chromatographic condition sample introduction, with isorhamnetin as reference
Peak, calculates relative retention time and the peak area ratio at total peak.Result shows the relative retention time RSD ＜ at each total peak
0.12%, relative peak area RSD ＜ 1.75%, show that instrument precision is good.
2.3 replica test
Take with a collection of test sample 5 parts, prepare need testing solution by preparation method, measure by chromatographic condition sample introduction, with isorhamnetin
For with reference to peak, calculating relative retention time and the peak area ratio at each total peak.Result shows when relatively retaining of each total peak
Between RSD ＜ 1.01%, relative peak area RSD ＜ 2.05%, show that analysis method repeatability is good.
2.4 stability test
Take with a collection of need testing solution, by chromatographic condition, respectively at 0 h, 5 h, 10 h, 15 h, 20 h, 25 h sample introductions, record
Chromatogram, with isorhamnetin for reference to peak, calculating relative retention time and the peak area ratio at total peak.Result shows each total
The relative retention time RSD ＜ 0.09% at peak, relative peak area RSD ＜ 2.11 %, shows that need testing solution room temperature is placed on 25h
Internal stability is good.
2.5 similarity evaluation
Use " similarity evaluation (2004A version) ", use Supplements that 100 batches of collection of illustrative plates are carried out
Coupling, calculates similarity, and median method generates reference fingerprint, as shown in Figure 2.Being computed, sample room similarity is 0.964
Above, the reference fingerprint similarity of each batch sample and generation is all between 0.974 ~ 0.999.Show silver yellow between each batch
There is some difference for grain, but technique is more stable generally, and product homogeneity is preferable, and the method can relatively be used on Yinhuang Particle quality
Control.
Claims (5)
1. the assay method of a Yinhuang Particle finger printing, it is characterised in that comprise the following steps:
(1) preparation of reference substance solution: precision weighs isorhamnetin, baicalin, baicalin, luteoloside, 4-dicaffeoylquinic acid, fresh green
Ortho acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, oroxylin, chrysin, wogonoside, wogonin, add first respectively
Alcohol dissolves, and adds isopyknic water, is respectively prepared 0.1mg/ml reference substance solution；
(2) preparation of inner mark solution: precision weighs isorhamnetin, adds methanol and dissolves, add isopyknic water, and constant volume becomes concentration
It is 30 g mL-1Inner mark solution；
(3) need testing solution preparation method: take Yinhuang Particle, add methanol solution making concentration is 40mg mL-1Sample solution；
By sample solution and 30 g mL-1Inner mark solution equal-volume mixing, through 0.22 m microporous filter membrane filter, take subsequent filtrate as confession
Test sample solution；
(4) measure: utilize HPLC MS to be analyzed measuring.
Finger print measuring method the most according to claim 1, it is characterised in that High Performance Liquid Chromatography condition
For: Agela Venusil MP C18(4.6mm × 250mm, 5 m) for chromatographic column；Condition is: column temperature 30 DEG C, flow velocity 1.0 mL
min-1, detecting wavelength 235nm, sample size is: 10 μ L, and with acetonitrile as mobile phase A, volume fraction is that 0.2% phosphate aqueous solution is for flowing
Dynamic phase B, volume fraction be 0.5% phosphate aqueous solution carry out gradient elution for flowing phase C.
Finger print measuring method the most according to claim 2, it is characterised in that the condition of gradient elution is:
0-10 min, 5-9% mobile phase A, 95-91% Mobile phase B；10-31 min, 9-16% mobile phase A, 91-84% Mobile phase B；
31-42 min, 16% mobile phase A, 84% Mobile phase B；42-65 min, 16-20% mobile phase A, 84-80% Mobile phase B；65-
90min, 20-22% mobile phase A, 80-78% Mobile phase B；90-120min, 22% mobile phase A, 78% flowing phase C；120-150min,
22-25% mobile phase A, 78-75% flows phase C；150-170min, 25-32% mobile phase A, 75-68% flows phase C；170-
185min, 32-45% mobile phase A, 68-55% flows phase C；185-200 min, 45-60% mobile phase A, 55-40% flows phase C；
200-220 min, 60-80% mobile phase A, 40-20% flows phase C；220-250min, 80-100% mobile phase A, 20-0% flows phase
C；
Described percentage ratio is percent by volume.
Finger print measuring method the most according to claim 1, it is characterised in that the condition of mass spectrography is: use ESI from
Component, negative ions alternative scanning mode；Ion strap mass analyzer, mass scan range: 50～1500 m/z；Scanning speed
26000 m/z•s-1；Spray pressure power 35.0psi；It is dried temperature 350 DEG C；Dry gas stream speed 9L min-1；Capillary tube electricity
Press 4000 V；Collision gas: helium.
5. according to the finger print measuring method one of claim 1-4 Suo Shu, it is characterised in that in step (3), test sample is molten
The preparation method of liquid is: take Yinhuang Particle, and precision weighs fine powder 1.0g, is placed in 50 mL round-bottomed flasks, accurate addition volume integral
Number is 50% methanol aqueous solution 25mL, weighs, is heated to reflux 20min, lets cool, and mends weight, filters, obtains subsequent filtrate 1；Take subsequent filtrate 1 with
Inner mark solution equal-volume mixes, and filters through 0.22 m microporous filter membrane, obtains subsequent filtrate 2 as need testing solution.
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Application publication date: 20160831 |