CN105954311A - Method for constructing <1>H-NMR fingerprint spectra of Periplaneta americana and extract of Periplaneta americana - Google Patents
Method for constructing <1>H-NMR fingerprint spectra of Periplaneta americana and extract of Periplaneta americana Download PDFInfo
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Abstract
The invention discloses a method for constructing <1>H-NMR fingerprint spectra of Periplaneta americana and an extract of the Periplaneta americana. According to the method, a Periplaneta americana medicinal material and 15 compounds in an extract of the Periplaneta americana medicinal material are obtained by virtue of a nuclear magnetic resonance technique, and the 15 compounds include 3 nucleoside components and 12 amino acid components. Compared with traditional chromatographic methods such as HPLC, the method has the advantages that more comprehensive information can be provided, and the nucleoside components and the amino acid components can be simultaneously analyzed by virtue of single measurement. According to the method, a <1>H-NMR-based metabonomics technique is creatively utilized, the integral chemical components of the Periplaneta americana and the extract are simultaneously detected for the first time, and the masses of the Periplaneta americana and the extract can be comprehensively controlled by virtue of finally constructed <1>H-NMR fingerprint spectra, thereby providing scientific basis for the variety identification of the Periplaneta americana and the mass control of the extract of the Periplaneta americana in future.
Description
Technical field
The present invention relates to the method for quality control of a kind of Chinese crude drug, particularly to periplaneta americana and extract1H-NMR refers to
The construction method of stricture of vagina collection of illustrative plates.
Background technology
Periplaneta americana (Periplaneta americana) is recorded in Shennong's Herbal the earliest, is classified as middle product, has work
Blood is promoted blood circulation, effect of inducing diuresis to remove edema, expelling pus and promoting granulation, is mainly used in treating that lump in the abdomen, children's's cellulitis be long-pending and the disease such as sore and toxic.Mesh
Before in the document reported, the quality control of periplaneta americana and extract thereof mainly becomes with one or more nucleoside, amino acids
It is divided into index to carry out assay research.This " Points replacing surfaces " mode does not meets the entirety of Chinese medicine multicomponent, Mutiple Targets undoubtedly
Property function Characteristics.Periplaneta americana medical material and the quality evaluation of extract and control method thereof should be based on the changes analyzing its entirety
Study packet, rather than only analyze wherein one or more compositions.And use1H-NMR metabonomic technology, system carries out America
The quality controling research of big Lian and extract thereof there is no report so far.
Summary of the invention
By research, novelty use based on1The metabonomic technology of H-NMR, makes full use of it and embodies globality, sample
Preparation is simple, the analysis time of the methodology advantage such as quickly, finally sets up periplaneta americana and extract thereof1H-NMR finger printing,
Can be as measuring the method for chemical constituent in periplaneta americana medical material and extract, it is possible to as identifying periplaneta americana medical material and carrying
Take material amount control method.Scientific basis is provided for the cultivar identification of periplaneta americana from now on and the quality control of extract thereof.
The nuclear magnetic resonance map of periplaneta americana medical material and extract thereof is studied by the present invention, it is provided that a kind of quickly,
Easy periplaneta americana and extract thereof1H-NMR fingerprint map construction method, compares with tradition HPLC isochromatic spectrum method, this
Invention can provide more comprehensively information, and single measurement just can analyze nucleoside and Amino acids simultaneously.For periplaneta americana
Medical material and the detection of extract total quality thereof lay the foundation.
A kind of periplaneta americana medical material that the present invention provides1The construction method of H-NMR finger printing, the method includes following
Step:
Weigh dry periplaneta americana medicinal powder 0.1～1.0g, be placed in conical flask, be separately added into containing 3-(trimethyl
Silica-based) CD of deuterated sodium propionate (TSP) internal standard substance3OD and D2O dissolves, obtain the concentration of periplaneta americana medicinal powder be 0.1～
0.4g/mL, seals, and after supersound extraction 0.5～2h, crosses 0.45 μm microporous filter membrane, takes 0.6mL filtrate to the 5mm nuclear magnetic tube of standard
In, seal up, be directly used in1H-NMR measures；Nuclear magnetic tube is placed in nuclear magnetic resonance analyser, uses the presaturation pulse train of standard
Compacting water peak measures periplaneta americana medical material sample1H-NMR finger printing, wherein test parameter and condition are: use the pre-of standard
Saturation pulse sequence (zgpr) compacting water peak-to-peak signal, frequency internal lock is deuterated methanol, measures temperature 25 DEG C, observed frequency
400.13MHz, spectrum width 6393.9Hz, sampling time 4.089s, pulse delay time 4s, scanning times 128, pulse width 8.97
μ s, gathers data point 65536；
Wherein, CD3OD and D2The volume ratio of O solution is 1:1；KH2PO4Content be 12.32mg/mL.
Periplaneta americana medical material1On H-NMR finger printing, proton signal peak is distributed between δ 0-8.4, according to proton signal
A point situation is split in the chemical displacement value at peak and coupling, obtains each reference substance in conjunction with reference to pertinent literature1H-NMR spectral data, altogether
Identify 3 nucleoside compounds (numbering 1-3) and 12 amino-acid compounds (numbering 4-15), be shown in Table 1.
Chemical composition in table 1 periplaneta americana medical material1H-NMR belongs to
Measure American-cockroach-extract 0.5～3.0mL, be placed in evaporating dish, volatilize, be separately added into containing 3-(trimethyl silicane
Base) CD of internal standard substance of deuterated sodium propionate (TSP)3OD and D2O dissolves, and seals, and after ultrasonic dissolution, crosses 0.45 μm microporous filter membrane, takes
0.6mL filtrate, in the 5mm nuclear magnetic tube of standard, is sealed up, is directly used in1H-NMR measures；
Wherein, CD3OD and D2The volume ratio of O solution is 1:1；KH2PO4Content be 12.32mg/mL.Nuclear magnetic tube is placed in
In nuclear magnetic resonance analyser, the presaturation pulse train compacting water peak of standard is used to measure American-cockroach-extract sample1H-NMR fingerprint
Collection of illustrative plates, wherein test parameter and condition are: use presaturation pulse train (zgpr) the compacting water peak-to-peak signal of standard, frequency internal lock
For deuterated methanol, measuring temperature 25 DEG C, observed frequency 400.13MHz, spectrum width 6393.9Hz, sampling time 4.089s, pulse is prolonged
Time 4s late, scanning times 128, pulse width 8.97 μ s, gather data point 65536；
Periplaneta americana medical material1On H-NMR finger printing, proton signal peak is distributed between δ 0-8.4, according to proton signal
A point situation is split in the chemical displacement value at peak and coupling, obtains each reference substance in conjunction with reference to pertinent literature1H-NMR spectral data, altogether mirror
Make 3 nucleoside compounds (numbering 1-3) and 12 amino-acid compounds (numbering 4-15).It is shown in Table 2.
Table 2 periplaneta americana medicinal substances extract1H-NMR belongs to
Periplaneta americana medical material that the present invention builds and extract thereof1H-NMR finger printing, can characterize periplaneta americana simultaneously
15 kinds of chemical compositions in medical material and extract thereof, all can periplaneta americana medicinal substances extract make including but not limited to health
The productions such as multiple new liquid, rehabilitation new capsule, rehabilitation new film or quality testing are applied.Compare with traditional HPLC isochromatic spectrum method,
The present invention can provide more comprehensively information, and single measurement just can analyze nucleoside and Amino acids simultaneously.Described method
Sample preparation is simple, it is fast to analyze speed.Realizing periplaneta americana medical material and extract total quality context of detection has wide
Application prospect.
Accompanying drawing explanation
Fig. 1 periplaneta americana medical material is representational1H-NMR collection of illustrative plates.
Fig. 2 periplaneta americana medical material1Signals assignment (the low place of A of H-NMR collection of illustrative plates；Place in B；C high field region): 1 inosine；2
Hypoxanthine；3 uracil；4 glutamic acid；5 histidine；6 tryptophans；7 phenylalanine；8 proline；9 aspartic acids；10 essence ammonia
Acid；11 lysines；12 valines；13 glycine；14 alanine；15 leucines.
-7 five batches of periplaneta americana medical materials of Fig. 31H-NMR collection of illustrative plates.
Fig. 8 periplaneta americana medicinal substances extract is representational1H-NMR collection of illustrative plates.
Fig. 9 periplaneta americana medicinal substances extract1Signals assignment (the low place of A of H-NMR collection of illustrative plates；Place in B；C high field region): 1
Inosine；2 hypoxanthine；3 uracil；4 glutamic acid；5 histidine；6 tryptophans；7 phenylalanine；8 proline；9 aspartic acids；10
Arginine；11 lysines；12 valines；13 glycine；
14 alanine；15 leucines.
-14 five batches of periplaneta americana medicinal substances extracts of Figure 101H-NMR collection of illustrative plates.
Detailed description of the invention
Embodiment 1: periplaneta americana medical material1The foundation of H-NMR standard finger-print
1.1 instruments and reagent
Nuclear magnetic resonance chemical analyser Bruker AVANCE III 400M；Sartorius BP221S electronic balance (match by Beijing
Many Li Si scientific instrument company limited)；KQ-300B type ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.)；W201 type
Thermostat water bath (Shen Shun bio tech ltd, Shanghai)；Deuterated methanol (CD3OD, 99.8%)；Heavy water (D2O, 99.9%)；
3-(trimethyl is silica-based) deuterated sodium propionate (TSP) is purchased from Sigma-Aldrich (St.Louis, Mo, USA)；AG di(2-ethylhexyl)phosphate
Hydrogen potassium (KH2PO4) purchased from Chengdu Ke Long chemical reagent factory.
Periplaneta americana medical material is provided by Sichuan Haoyisheng Panxi Pharmaceutical Co., Ltd..
The preparation of 1.2 periplaneta americana medical material need testing solutions
Weigh dry periplaneta americana medicinal powder 0.2g, be placed in conical flask, be separately added into containing 3-(trimethyl is silica-based)
The CD of deuterated sodium propionate (TSP) internal standard substance3OD and D2O dissolves, CD3OD and D2The volume of O is respectively 0.7mL and 0.7mL, obtains
The concentration of periplaneta americana medicinal powder is 0.143g/mL, seals, and after supersound extraction 0.5h, crosses 0.45 μm microporous filter membrane, takes
0.6mL filtrate, in the 5mm nuclear magnetic tube of standard, is sealed up, is directly used in1H-NMR measures.
1.31The mensuration of H-NMR finger printing
Nuclear magnetic tube is placed in nuclear magnetic resonance analyser, uses the presaturation pulse train compacting water peak of standard to measure periplaneta americana
Extract sample1H-NMR finger printing, wherein test parameter and condition are: use the presaturation pulse train (zgpr) of standard
Compacting water peak-to-peak signal, frequency internal lock is deuterated methanol, mensuration temperature 25 DEG C, observed frequency 400.13MHz, spectrum width 6393.9Hz,
Sampling time 4.089s, pulse delay time 4s, scanning times 128, pulse width 8.97 μ s, gather data point 65536.
1.41The qualification at H-NMR finger printing proton signal peak
1H-NMR finger printing is after phasing, baseline correction and chemical shift correct, according to proton signal peak
A point situation is split in chemical displacement value and coupling, obtains each reference substance in conjunction with reference to pertinent literature1H-NMR spectral data (table 3) and
Need testing solution1H-NMR finger printing (Fig. 1, Fig. 2), identifies 3 nucleoside compounds and 12 amino acid compounds altogether
Thing.In detail1H-NMR ownership is shown in Table 4.
The each reference substance obtained in table 3 list of references1H-NMR spectral data
Chemical composition in table 4 periplaneta americana1H-NMR identifies
1.51H-NMR fingerprint similarity is analyzed
Take 5 batches of periplaneta americana medical material products to be measured, measure as stated above1H-NMR finger printing (Fig. 3-7).To record
's1H-NMR free damping (FID) signal imports MestReNova software and carries out fourier transform, and manually adjusts phase place and base
Line, corrects chemical shift on the basis of TSP (0ppm).To the collection of illustrative plates of 0.7-8.7ppm scope with 0.04ppm as chemical displacement value
Unit carries out subsection integral, and is normalized with total peak area, then exports data with ASCII fromat, obtains eachization
Displacement study section corresponding signal peak area value.This test obtains 200 sections of integrations altogether, then deducts 2 sections of letters belonging to methanol
Number (3.26-3.34ppm) and 4 sections of water peak-to-peak signals (4.74-4.90ppm), finally give 194 hop count strong points, with the standard formulated
Finger printing compares, and uses correlation coefficient process and included angle cosine value method to calculate qualitative similarity, and similarity is more than 0.95
Thinking qualified, result sees table 5.
As known from Table 5,5 batches of periplaneta americana medical material samples1The correlation coefficient of H-NMR finger printing is respectively 0.970,
0.998,0.973,0.990 and 0.998, meansigma methods is 0.986；Included angle cosine is respectively 0.979,0.998,0.981,0.992
With 0.998, meansigma methods is that the similarity of 0.9905 batch of periplaneta americana medical material is higher, is all higher than 0.970, and result shows between batch
Overall fingerprint feature similarity, also explanation is set up1H-NMR finger printing can detect the quality of periplaneta americana medical material well
Stability.
Table 5 is the similarity evaluation result of five batches of periplaneta americana samples
Embodiment 2: periplaneta americana medicinal substances extract1The foundation of H-NMR standard finger-print
1.1 instruments and reagent
Nuclear magnetic resonance chemical analyser Bruker AVANCE III 400M；Sartorius BP221S electronic balance (match by Beijing
Many Li Si scientific instrument company limited)；KQ-300B type ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.)；W201 type
Thermostat water bath (Shen Shun bio tech ltd, Shanghai)；Deuterated methanol (CD3OD, 99.8%)；Heavy water (D2O, 99.9%)；
3-(trimethyl is silica-based) deuterated sodium propionate (TSP) is purchased from Sigma-Aldrich (St.Louis, Mo, USA)；AG di(2-ethylhexyl)phosphate
Hydrogen potassium (KH2PO4) purchased from Chengdu Ke Long chemical reagent factory.Periplaneta americana medicinal substances extract is climbed Western medicine industry by the good doctor in Sichuan to be had
Limit responsible company provides.
The preparation of 1.2 periplaneta americana medicinal substances extract need testing solutions
Measure American-cockroach-extract 1.5mL, be placed in evaporating dish, volatilize, be separately added into containing 3-(trimethyl is silica-based) deuterium
CD for the internal standard substance of sodium propionate (TSP)3OD and D2O dissolves, and after ultrasonic dissolution, crosses 0.45 μm microporous filter membrane, takes 0.6mL filtrate
To the 5mm nuclear magnetic tube of standard, seal up, be directly used in1H-NMR measures.
1.31The mensuration of H-NMR finger printing
Nuclear magnetic tube is placed in nuclear magnetic resonance analyser, uses the presaturation pulse train compacting water peak of standard to measure periplaneta americana
Extract sample1H-NMR finger printing, wherein test parameter and condition are: use the presaturation pulse train (zgpr) of standard
Compacting water peak-to-peak signal, frequency internal lock is deuterated methanol, mensuration temperature 25 DEG C, observed frequency 400.13MHz, spectrum width 6393.9Hz,
Sampling time 4.089s, pulse delay time 4s, scanning times 128, pulse width 8.97 μ s, gather data point 65536.
1.41The qualification at H-NMR finger printing proton signal peak
1H-NMR finger printing is after phasing, baseline correction and chemical shift correct, according to proton signal peak
A point situation is split in chemical displacement value and coupling, obtains each reference substance in conjunction with reference to pertinent literature1H-NMR spectral data (table 3) and
Need testing solution1H-NMR finger printing (Fig. 8, Fig. 9), identifies 3 nucleoside compounds and 12 amino acid compounds altogether
Thing.In detail1H-NMR ownership is shown in Table 6.
Chemical composition in table 6 American-cockroach-extract1H-NMR identifies
1.51H-NMR fingerprint similarity is analyzed
Take 5 batches of American-cockroach-extract products to be measured, measure as stated above1H-NMR finger printing (Figure 10-14).Will
Record1H-NMR free damping (FID) signal imports MestReNova software and carries out fourier transform, and manually adjusts phase place
And baseline, on the basis of TSP (0ppm), correct chemical shift.To the collection of illustrative plates of 0.7-8.7ppm scope with 0.04ppm as chemical potential
Shifting value unit carries out subsection integral, and is normalized with total peak area, then exports data with ASCII fromat, obtains
Each chemical shift section corresponding signal peak area value.This test obtains 200 sections of integrations altogether, then deducts 2 sections and belong to methanol
Signal (3.26-3.34ppm) and 4 sections of water peak-to-peak signals (4.74-4.90ppm), finally give 194 hop count strong points, with formulate
Standard finger-print compares, and uses correlation coefficient process and included angle cosine value method to calculate qualitative similarity, and similarity is more than
Think qualified for 0.95.Result sees table 7.
As known from Table 7,5 batches of American-cockroach-extract samples1The correlation coefficient of H-NMR finger printing is respectively 0.990,
0.998,1.000,0.998 and 0.998, meansigma methods is 0.997；Included angle cosine is respectively 0.980,0.998,1.000,0.998
With 0.986, meansigma methods is 0.992.The similarity of 5 batches of American-cockroach-extract samples is higher (being all higher than 0.980), shows to be built
Stand1H-NMR finger printing can detect the quality stability of American-cockroach-extract sample well, also indicates that different batches
American-cockroach-extract difference in chemical constituents analysis ratio is little.
Table 7 is the similarity evaluation result of five batches of American-cockroach-extracts
Claims (10)
1. periplaneta americana1The construction method of H-NMR finger printing, the method comprises the following steps:
(A) preparation of periplaneta americana medical material sample solution
Weigh dry periplaneta americana medicinal powder 0.1～1.0g, be placed in conical flask, be separately added into containing 3-(trimethyl is silica-based)
The CD of deuterated sodium propionate (TSP) internal standard substance3OD and D2O dissolves, and the concentration obtaining periplaneta americana medicinal powder is 0.1～0.4g/
ML, seals, and after supersound extraction 0.5～2h, crosses 0.45 μm microporous filter membrane, takes 0.6mL filtrate in the 5mm nuclear magnetic tube of standard, adds
Envelope, is directly used in1H-NMR measures；
(B)1The mensuration of H-NMR finger printing
Nuclear magnetic tube is placed in nuclear magnetic resonance analyser, uses the presaturation pulse train compacting water peak of standard to measure periplaneta americana medical material
Sample1H-NMR finger printing, wherein test parameter and condition are: use presaturation pulse train (zgpr) the compacting water of standard
Peak-to-peak signal, frequency internal lock is deuterated methanol, measures temperature 25 DEG C, and observed frequency 400.13MHz, spectrum width 6393.9Hz, during sampling
Between 4.089s, pulse delay time 4s, scanning times 128, pulse width 8.97 μ s, gather data point 65536；
(C) qualitative identification at proton signal peak
Periplaneta americana medical material1On H-NMR finger printing, proton signal peak is distributed between δ 0-8.4, according to proton signal peak
A point situation is split in chemical displacement value and coupling, and combines with reference to the pertinent literature each reference substance of acquisition1H-NMR spectral data, altogether mirror
Make 3 nucleoside compounds and 12 amino-acid compounds.
A kind of periplaneta americana medical material the most according to claim 11The construction method of H-NMR finger printing, it is characterised in that
The preparation method of described step (A) Central America big Lian medical material sample solution is: weigh dry periplaneta americana medicinal powder 0.2g,
It is placed in conical flask, is separately added into the CD containing 3-(trimethyl is silica-based) deuterated sodium propionate (TSP) internal standard substance3OD and D2O dissolves,
CD3OD and D2The volume of O is respectively 0.7mL and 0.7mL, and the concentration obtaining periplaneta americana medicinal powder is 0.143g/mL, seals,
After supersound extraction 0.5h, cross 0.45 μm microporous filter membrane, take 0.6mL filtrate in the 5mm nuclear magnetic tube of standard, seal up, be directly used in1H-NMR measures.
A kind of periplaneta americana medical material the most according to claim 1 and 21The construction method of H-NMR finger printing, its feature
It is: CD3OD and D2The volume ratio of O solution is 1:1.
A kind of periplaneta americana medical material the most according to claim 1 and 21The construction method of H-NMR finger printing, its feature
It is: CD3OD and D2Possibly together with KH in O solution2PO4, its content is 12.32mg/mL.
A kind of periplaneta americana medical material the most according to claim 11H-NMR fingerprint map construction method, it is characterised in that:
In described step (C), 3 nucleoside compounds (numbering 1-3) and 12 amino-acid compounds (numbering 4-15) are respectively as follows:
6. an American-cockroach-extract1The construction method of H-NMR finger printing, the method comprises the following steps:
(A) preparation of American-cockroach-extract sample solution
Measure American-cockroach-extract 0.5～3.0mL, be placed in evaporating dish, volatilize, be separately added into containing 3-(trimethyl is silica-based) deuterium
CD for the internal standard substance of sodium propionate (TSP)3OD and D2O dissolves, and seals, and after ultrasonic dissolution, crosses 0.45 μm microporous filter membrane, takes 0.6mL
Filtrate, in the 5mm nuclear magnetic tube of standard, is sealed up, is directly used in1H-NMR measures；
(B)1The mensuration of H-NMR finger printing
Nuclear magnetic tube is placed in nuclear magnetic resonance analyser, uses the presaturation pulse train compacting water peak of standard to measure periplaneta americana and extract
Thing sample1H-NMR finger printing, wherein test parameter and condition are: use presaturation pulse train (zgpr) compacting of standard
Water peak-to-peak signal, frequency internal lock is deuterated methanol, measures temperature 25 DEG C, observed frequency 400.13MHz, spectrum width 6393.9Hz, sampling
Time 4.089s, pulse delay time 4s, scanning times 128, pulse width 8.97 μ s, gather data point 65536；
(C) qualitative identification at proton signal peak
American-cockroach-extract1On H-NMR finger printing, proton signal peak is distributed between δ 0-8.4, according to proton signal peak
Chemical displacement value and coupling split a point situation, obtain each reference substance in conjunction with reference to pertinent literature1H-NMR spectral data, altogether mirror
Make 3 nucleoside compounds and 12 amino-acid compounds.
A kind of periplaneta americana medicinal substances extract the most according to claim 61The construction method of H-NMR finger printing, it is special
Levy and be that the preparation method of described step (A) Central America big Lian extract sample solution is: measure American-cockroach-extract
1.5mL, is placed in evaporating dish, volatilizes, and is separately added into internal standard substance containing 3-(trimethyl is silica-based) deuterated sodium propionate (TSP)
CD3OD and D2O dissolves, CD3OD and D2The volume of O is respectively 0.7mL and 0.7mL, seals, and after ultrasonic dissolution, crosses 0.45 μm micropore
Filter membrane, takes 0.6mL filtrate in the 5mm nuclear magnetic tube of standard, seals up, be directly used in1H-NMR measures.
8. according to a kind of periplaneta americana medicinal substances extract described in claim 6 or 71The construction method of H-NMR finger printing,
It is characterized in that: CD3OD and D2The volume ratio of O solution is 1:1.
9. according to a kind of periplaneta americana medicinal substances extract described in claim 6 or 71The construction method of H-NMR finger printing,
It is characterized in that: CD3OD and D2Possibly together with KH in O solution2PO4, its content is 12.32mg/mL.
A kind of periplaneta americana medicinal substances extract the most according to claim 61H-NMR fingerprint map construction method, it is special
Levy and be: 3 nucleoside compounds (numbered 1-3) and 12 amino-acid compounds (numbered 4-15) in described step (C)
It is respectively as follows:
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| CN109651332A (en) * | 2017-10-12 | 2019-04-19 | 四川好医生攀西药业有限责任公司 | The preparation method and applications of Dopaminergics derivative |
| CN109959732A (en) * | 2017-12-26 | 2019-07-02 | 内蒙古京新药业有限公司 | The separation method of Kangfuxin Liquid finger-print and its effective constituents A |
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