CN107389721B - A method of based on NMR technology fast quantification active Chinese drug component component - Google Patents

A method of based on NMR technology fast quantification active Chinese drug component component Download PDF

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CN107389721B
CN107389721B CN201710562518.8A CN201710562518A CN107389721B CN 107389721 B CN107389721 B CN 107389721B CN 201710562518 A CN201710562518 A CN 201710562518A CN 107389721 B CN107389721 B CN 107389721B
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CN107389721A (en
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陈福欣
龚频
陈苏英
侯彬彬
严贝贝
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Xian University of Science and Technology
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Abstract

The present invention provides a kind of method based on NMR technology fast quantification active Chinese drug component component: 1) sample being dissolved in deuterated reagent and be transferred to nuclear magnetic tube, internal standard compound is added into nuclear magnetic tube；2) using the hydrogen resonant frequency sampling in NMR；3) the feature structure signal peak and internal standard compound signal peak for choosing tested component calculate tested constituent content using inner mark method ration.The present invention selects NMR technology to detect the content of Chinese medicine active component, can carry out fast quantitative analysis to active component in or mixtures thereof Chinese medical extract, initial gross separation compound and natural origin small molecule compound etc., provide molar content.The present invention has the features such as easy to operate, rapid batch is realized, favorable reproducibility is tested, and experimental data is intuitive and reliable, the detection especially suitable for micro-example；The idea and method of a fast quantification is provided for the research of the effective substance of Chinese medicine or compound.

Description

A method of based on NMR technology fast quantification active Chinese drug component component
Technical field
The present invention relates to a kind of methods based on NMR technology fast quantification active Chinese drug component component, belong to Chinese pharmacology field.
Background technique
The effective substance research of Chinese medicine is the key problem during the modernization of Chinese medicine.Traditional " separation-identification- Natural Medicine Chemistry research mode heavy workload, the low separation efficiency of screening "；Meanwhile complicated component and effective substance content phase The difficulty that effective substance research is increased to low feature, also limits the paces of the modernization of Chinese medicine.At the same time, modern pharmacology Structure activity study then needs clearly to know the content of active material.Activity guiding TCM in Vitro rapid screening method be One of important method of the modernization of Chinese medicine.This method uses vitro enzyme or cell model for work using specific pharmacological activity as target Tool, targetedly optimizes separation condition, is quickly obtained active Chinese drug component component and the active preliminary Quantitative Structure effect of specific pharmacology is closed It is (QSAR).In short, how to obtain micro or even trace active constituent quantitative information has important meaning to the modernization of Chinese medicine Justice.
HPLC-UV and HPLC-MS/MS is the common method of Chinese medicine microcomponent quantitative analysis, however in complexity For medicine component, both methods has certain limitation.HPLC-UV is suitable for quantitative point of the stronger compound of UV absorption The sensitivity of analysis, analysis is poor, and due to the difference of compound molar extinction coefficient, compound quantitative determination is needed with mark Quasi- sample makes standard curve, and then obtains the content of measured matter, for complicated traditional Chinese medicinal components, draws each The standard curve of compound is clearly very bothersome and unpractical, and many ingredients or unknown.Therefore, the party Method is relatively high suitable for content and has the assay of the known compound of UV absorption.HPLC-MS/MS is that sensitivity is non- Chang Gao, and the wider quantitative approach of the scope of application.No matter whether compound has UV absorption, and available this method measurement contains Amount, the micro quantitative analysis to trace materials being commonly used in research complex matrices.It is equally needed when with external standard method content Standard sample is wanted to draw standard curve, disadvantage is as HPLC-UV.Standard items are not needed when with internal standard method, but are needed Want internal standard compound identical as the correction factor of measured matter, due to the limitation of MS principle, under the same terms, different types of structure chemical combination The degree of ionization of object has a very big difference, and correction factor difference is equally very big, can not find a kind of internal standard compound and come while surveying Determine the compound of different types of structure.
In view of the above analysis, for the same of same characteristic features structure in the structure activity study of Chinese medicine modern pharmacology Quick, the accurate quantitative analysis of a kind of active component are one and need urgent problem to be solved.
Summary of the invention
The purpose of the present invention is to provide a kind of methods based on NMR technology fast quantification active Chinese drug component component.
In order to achieve the above objectives, the invention adopts the following technical scheme:
1) traditional Chinese medicine sample is dissolved in after deuterated reagent be transferred to nuclear magnetic tube (nuclear magnetic tube for example selected from outer diameter be 1.7mm, The quartzy or high borosilicate nuclear magnetic tube of 2.1mm or 5mm), internal standard compound then is added into the nuclear magnetic tube, obtains analysis sample；
2) sample detection is completed to analysis sample by using the hydrogen resonant frequency in NMR；
3) the hydrogen resonance signal obtained according to sampling chooses signal peak corresponding with the feature structure of tested component and internal standard Certain characteristic signal peak of object calculates tested constituent content using inner mark method ration, and the tested component refers to can be according to described Some or certain a kind of active material that other active materials distinguish in feature structure and the traditional Chinese medicine sample.
The method of the quantitative active Chinese drug component component is further comprising the steps of: after the completion of sample detection, to the analysis sample The nonelectrolyte mixed aqueous solution that can be dissolved each other with the deuterated reagent is added in product, then passes through refrigerated centrifuge concentration and recovery traditional Chinese medicine sample.
The traditional Chinese medicine sample is selected from Chinese medicine material medicament extract, compound Chinese medicinal preparation, the compound obtained through separation means Or mixtures thereof, the small molecule compound of natural origin small molecule compound or synthesis；Traditional Chinese medicine sample institute's expense is 1 in detection ~100mg.
The deuterated reagent is selected from CDCl3、DMSO-d6、CD3OD、acetone-d6、THF-d8、DMSO-d6、benzene- d6、toluene-d8、D2O、pyridine-d5Or acetonitrile-d3；The dosage of deuterated reagent is in traditional Chinese medicine sample dissolution 0.3~0.6mL.
The internal standard compound be selected from trans-dichloroethylene, cis- dichloroethylene, trichloro ethylene, paracide, to difluorobenzene, One or more of trifluoro-benzene, 1,2,3,4- phenyl tetrafluoride, 1,2,4,5- phenyl tetrafluoride, 1,3,4,5- phenyl tetrafluoride, phenyl-pentafluoride Combination；Solution is made with the deuterated reagent in advance before nuclear magnetic tube is added in the internal standard compound, and the dosage of the solution is 1~10 μ L, and internal standard compound total concentration is 0.1~1M.
In the sampling, the angle of pulse train is 30~90 degree, and relaxation time >=5s, scanning times are 32~1024 Secondary, probe temperature is 20~40 DEG C, spectral peak width≤20ppm, preferably 0~10ppm.
The corresponding signal peak of the feature structure, is selected from double bond at the peak s, d, dd, t or m of 6.1~6.5ppm of δ, for Methoxyl group be selected from 3.6~4.2ppm of δ the peak s, for aromatic ring be selected from 6.5~7.5ppm of δ the peak s or d, for aldehyde be selected from δ 7.5~ The peak s of 9.5ppm is selected from acid at the peak s of 9.5~12.5ppm of δ, is selected from δ 4.5 for acetal, ketal, hemiacetal and hemiketal The peak s of~6.5ppm.
Molar content of the tested component in the traditional Chinese medicine sample is calculated according to following formula:
MIt is living=cMark×VMark×AIt is living×fMark/(AMark×fIt is living)=MMark×AIt is living×fMark/(AMark×fIt is living) (1)
In formula (1), MIt is livingFor the molal quantity for being tested component；MMarkFor the molal quantity of internal standard compound；cMarkFor rubbing for added internal standard compound That concentration, VMarkFor the volume number of added internal standard compound；AIt is livingFor the peak area of the corresponding signal peak of the feature structure；AMarkFor selection The peak area at internal standard compound characteristic signal peak, fMarkFor the peak area at unit molal quantity internal standard compound characteristic signal peak, fIt is livingFor unit mole The peak area of the tested corresponding signal peak of component characteristics structure of number.
The dosage of the mixed solvent is 10~100 times for analyzing sample volume, and the water content of the mixed solvent presses body Fraction meter >=80%；The condition of the refrigerated centrifuge are as follows: centrifugal rotational speed is 500~4000rpm, and sample room temperature is 20~60 DEG C, cryogenic temperature≤- 20 DEG C, the time be 2~for 24 hours.
The beneficial effects of the present invention are embodied in:
The present invention, can be to change using NMR using the hydrogen resonant frequency of NMR method measurement internal standard compound and active Chinese drug component component It closes different structure in object and carries out qualitative and quantitative feature, other in traditional Chinese medicine sample are different to tested component by internal standard method and are lived Property substance chemical structure characteristic carry out quantitative analysis, can be fast under the premise of unknown compound or mixture mole Speed, the molar content for accurately providing tested component, solve for the same class natural active products with same characteristic features structure The problem of the quick of matter, accurate quantitative analysis, is conducive to the quantitative comparison of screening active ingredients；The present invention have it is easy to operate, quickly The features such as batch is realized, favorable reproducibility is tested, and experimental data is intuitive and reliable is Chinese medicine especially suitable for the detection of micro-example Or the effective substance research of compound provides the idea and method of a fast quantification.
Further, quantitative analysis method of the invention is a kind of nondestructive analysis method, and mixing is added after sample detection is complete Solvent, by refrigerated centrifuge concentration and recovery, the sample rate of recovery is high, and is not influenced by internal standard compound, for precious sample (example Such as, the small molecule compound of or mixtures thereof compound obtained through separation means, natural origin small molecule compound or synthesis) Next step screening active ingredients provide convenience, reduce the time loss and cost of drug research.
Further, the peak area ratio that the present invention passes through the signal peak of feature structure in internal standard compound signal peak and tested component Value carrys out quantitative analysis and is tested component, and in conjunction with a large amount of traditional Chinese medicine fingerprint data, the internal standard compound screened has natural active products The structure feature that matter does not have, to (not need to carry out peak face when quantitatively calculating with natural active matter characteristic signal overlap of peaks Product is sought, and the signal peak for partly overlapping and being all overlapped is not used to quantitatively, therefore requires the signal peak of the two that can separate), And the chemical displacement value of internal standard compound itself only corresponds to a characteristic absorption peak, can realize under the limitation of internal standard compound dosage tested Quick, the accurate quantitative analysis of component.In addition, refrigerated centrifuge has been used in test sample recycling, and therefore, the screening of internal standard compound The requirement of test sample recycling is taken into account, i.e. the boiling point of internal standard compound needs lower, usually less than the boiling point of water, if being more than the boiling of water Point, then must assure that can separate in refrigerated centrifuge.
Further, the present invention passes through angle, relaxation time, scanning times, the probe temperature etc. in optimization pulse train Parameter eliminates influence of the signal peak drift to quantitative result so that the present invention is generally applicable in the quantitative of natural activity component, It is approached on peak position without requiring internal standard compound signal peak and the signal peak of tested component characteristics structure, quantifies active component more It is flexible, more accurate.
In addition, after the autosampler for combining NMR, unattended fast quantification is may be implemented in the present invention, people is saved Power, material resources.
Detailed description of the invention
Fig. 1 is Radix Gentianae Macrophyllae extract1HNMR map.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
The quantitative analysis of iridoid in 1 Radix Gentianae Macrophyllae extract of embodiment
Chinese medicine gentianae macrophyllae clinical application is extensive, is one of the main ingredient for treating rheumatic arthritis, tuberculosis hectic fever, yellow subcutaneous ulcer etc..And Iridoid constituents are the main actives of Chinese medicine gentianae macrophyllae.
(1) quantitative analysis step and result
Radix Gentianae Macrophyllae extract (Xi'an biotech firm, Tianrui, 75% ethanol extract) 100mg is dissolved in 0.5mL deuterated chloroform (CDCl3), it is transferred to 5mm standard nuclear magnetic tube, adds 5 μ L trichloro ethylene solution (solvent is deuterated chloroform, 1M), Bruker 400MHz measures the hydrogen resonance signal of sample, pops one's head in 24 DEG C of temperature control, calls pulse train zg (90 degree of pulse angles), redefines Relaxation time d1=5s, scanning times ns=32；Other parameters are standard parameter in sequence (for example, spectral peak width is 20ppm), Topspin 3.5 acquires data (Fig. 1).The qualitative of iridoid uses δ in Radix Gentianae Macrophyllae extract 6.32ppm (peak d), feature structure are double bond, CDCl3Reference hydrogen signal be δ 7.26ppm, s (correction δ value).Internal standard compound reference Peak is the hydrogen signal δ 6.65ppm (peak s) of trichloro ethylene, selects the reason of trichloro ethylene is as internal standard compound: 1) organizing a dtex with tested Sign architecture signals peak is not overlapped；2) peak position is close；3) meet internal standard compound dosage (concentration) limitation, achievable quantitative analysis；4) Boiling point is lower, is easy to remove in the concentration of following refrigerated centrifuges.The molal quantity of iridoid is calculated according to formula (1) Are as follows:
The μ L/100=0.05 μm of 1M × 5 ol
It is 0.5 μm of ol/g according to the content that iridoid in Radix Gentianae Macrophyllae extract is calculated in molar content.
After the completion of analysis, sample in nuclear magnetic tube is poured into 20mL and contains the mixed of 80% (volume) water and 20% (volume) ethyl alcohol In bonding solvent, refrigerated centrifuge concentration, centrifugal rotational speed 2000rpm, sample room temperature is 40 DEG C, and cryogenic temperature is -40 DEG C, concentration Time is 12h.Sample transfer is weighed and is re-started after refrigerated centrifuge1HNMR analysis, the results show that recycles in sample room consolidates Shape object weight 98.2mg has consistent finger-print (without deuterated reagent and internal standard compound) with Radix Gentianae Macrophyllae extract, and the rate of recovery reaches 98.2%.
(2) precision, reproducibility and stability experiment
1. Precision Experiment: taking 1 part of sample prepared, according to the method described above continuous sampling 5 times, automatic integration, to peak It is analyzed, the RSD of chemical shift and relative peak area between 0-0.31% and 0.1%-0.78%, illustrates the party respectively Method precision is good.
2. reproducibility is tested: taking with 5 parts of a batch of sample, sample 5 times according to the method described above.Automatic integration, to peak into The RSD of row analysis, chemical shift and relative peak area between 0-0.33% and 0.6%-1.22%, illustrates this method respectively Reproducibility is good.
3. stability experiment: 1 part of sample prepared is taken, respectively in 0,2,8,16,24,48h sampling determination, automatic product Point, peak is analyzed, the RSD of chemical shift and relative peak area is respectively less than 1.5%, illustrates that this method measures in 48h It is stable.
The quantitative analysis of paeoniflorin compound in 2 guizhi fuling pill of embodiment
Guizhi fuling pill prescription derives from " Synopsis Golden Chamber " of Eastern Han Dynasty's Zhang Zhongjing, is the normal of current treatment gynaecology's blood stasis disease Medication.Paeoniflorin compound is both one of the key factor of its active constituent and Quality Control.
(1) quantitative analysis step and result
Guizhi fuling pill 20mg is dissolved in 0.5mL deuterated methanol (CD3OD), it is transferred to 5mm standard nuclear magnetic tube, adds 10 μ L Phenyl-pentafluoride solution (solvent is deuterated methanol, 0.1M), Bruker 400MHz measure the hydrogen resonance signal of sample, temperature control 40 of popping one's head in DEG C, it calls pulse train zg30 (30 degree of pulse angles), redefines relaxation time d1=5s, scanning times ns=1024；Its His parameter is the standard parameter (for example, spectral peak width is 20ppm) in sequence, and Topspin 3.5 acquires data.Guizhi fuling pill The qualitative of middle paeoniflorin compound uses δ 5.31ppm (peak s), and feature structure is the c h bond of ketal in Paeoniflorin, internal standard compound Reference peak is the hydrogen signal δ 6.41ppm (s) of phenyl-pentafluoride.CD3The reference hydrogen signal of OD is δ 3.31ppm, s (correction δ value).According to The molal quantity of formula (1) calculating paeoniflorin compound are as follows:
μ L × the 0.12/0.85=0.14 μm of 0.1M × 10 ol
It is 7.05 μm of ol/g according to the content that paeoniflorin compound in guizhi fuling pill is calculated in molar content.
After the completion of analysis, sample in nuclear magnetic tube is poured into 10mL and contains the mixed of 90% (volume) water and 10% (volume) methanol In bonding solvent, refrigerated centrifuge concentration, centrifugal rotational speed 4000rpm, sample room temperature is 60 DEG C, and cryogenic temperature is -50 DEG C, concentration Time is 12h.Sample transfer is weighed and is re-started after refrigerated centrifuge1HNMR fingerprint map analyzing, the results show that in sample room The solid content weight 18.6mg of recycling has consistent finger-print (without deuterated reagent and internal standard compound) with guizhi fuling pill, returns Yield is up to 93%.
(2) precision, reproducibility and stability experiment are similar to Example 1, meet the validation criteria of methodology.
Above embodiments 1-2 is not the whole embodiments that this patent can be implemented, and the drug effect in Chinese medicine or compound is (living Property) material component content is low but structure is complicated, the present invention is targeted be one kind in Chinese medicine or compound with feature structure or Several compounds, the characteristic signal shared according to its HNMR is come quantitative analysis, different type in different Chinese medicine or Same Chinese Herbal Medicine The analysis condition of compound be all different, obtain the condition and range in the present invention accordingly.
The present invention selects NMR technology to detect the effective substance component content in Chinese medicine or compound, is to solve The problem of complicated ingredient is difficult to quantitative detection in actual production, scientific research, to various Chinese medical extracts, initial gross separation (such as through Chromatography etc.) or mixtures thereof compound and natural origin small molecule compound or the small molecule compound of synthesis can fast quantification Analysis, provides molar content.With easy to operate, rapid batch realization, favorable reproducibility, the intuitive and reliable equal spies of experimental data are tested Point, the detection especially suitable for micro-example；And sample can be recycled, the screening active ingredients of its next step are not influenced, application is wide, The idea and method of a fast quantification is provided for the research of the effective substance of Chinese medicine or compound.

Claims (7)

1. a kind of method based on NMR technology fast quantification active Chinese drug component component, it is characterised in that: the quantitative active Chinese drug component component Method the following steps are included:
1) traditional Chinese medicine sample is dissolved in after deuterated reagent and is transferred to nuclear magnetic tube, internal standard compound then is added into the nuclear magnetic tube, obtains Analyze sample；The internal standard compound be selected from trans-dichloroethylene, cis- dichloroethylene, trichloro ethylene, paracide, to difluorobenzene, Between one or both of trifluoro-benzene, 1,2,3,4- phenyl tetrafluoride, 1,2,4,5- phenyl tetrafluoride, 1,3,4,5- phenyl tetrafluoride, phenyl-pentafluoride with On combination；
2) sample detection is completed to analysis sample by using the hydrogen resonant frequency in NMR；
3) the hydrogen resonance signal obtained according to sampling, selection signal peak corresponding with the feature structure of tested component and internal standard compound Characteristic signal peak calculates tested constituent content using inner mark method ration, and the tested component refers to can be according to the feature knot Some or certain a kind of active material that other active materials distinguish in structure and the traditional Chinese medicine sample；The feature structure is corresponding Signal peak, the peak s, d, dd, t or m of 6.1~6.5ppm of δ is selected from for double bond, δ 3.6~4.2ppm is selected from for methoxyl group The peak s is selected from aromatic ring at the peak s or d of 6.5~7.5ppm of δ, and the peak s of 7.5~9.5ppm of δ is selected from for aldehyde, is selected from δ for acid The peak s of 9.5~12.5ppm is selected from acetal, ketal, hemiacetal and hemiketal at the peak s of 4.5~6.5ppm of δ；
The method of the quantitative active Chinese drug component component is further comprising the steps of: after the completion of sample detection, into the analysis sample The nonelectrolyte mixed aqueous solution that can be dissolved each other with the deuterated reagent is added, traditional Chinese medicine sample, the mixing are then recycled by refrigerated centrifuge The water content of solvent presses volume fraction >=80%.
2. a kind of method based on NMR technology fast quantification active Chinese drug component component according to claim 1, it is characterised in that: The traditional Chinese medicine sample is selected from Chinese medicine material medicament extract, compound Chinese medicinal preparation, the compound obtained through separation means or its mixing The small molecule compound of object, natural origin small molecule compound or synthesis；Traditional Chinese medicine sample institute's expense is 1~100mg in detection.
3. a kind of method based on NMR technology fast quantification active Chinese drug component component according to claim 1, it is characterised in that: The deuterated reagent is selected from CDCl3、DMSO-d6、CD3OD、acetone-d6、THF-d8、DMSO-d6、benzene-d6、 toluene-d8、D2O、pyridine-d5Or acetonitrile-d3；The dosage of deuterated reagent is 0.3 in traditional Chinese medicine sample dissolution ~0.6mL.
4. a kind of method based on NMR technology fast quantification active Chinese drug component component according to claim 1, it is characterised in that: Solution is made with the deuterated reagent in advance before nuclear magnetic tube is added in the internal standard compound, and the dosage of the solution is 1~10 μ L, and interior Mark object total concentration is 0.1~1M.
5. a kind of method based on NMR technology fast quantification active Chinese drug component component according to claim 1, it is characterised in that: In the sampling, the angle of pulse train is 30~90 degree, and relaxation time >=5s, scanning times are 32~1024 times, probe temperature Degree is 20~40 DEG C, spectral peak width≤20ppm.
6. a kind of method based on NMR technology fast quantification active Chinese drug component component according to claim 1, it is characterised in that: Molar content of the tested component in the traditional Chinese medicine sample is calculated according to following formula:
MIt is living=MMark×AIt is living×fMark/(AMark×fIt is living)
In formula, MIt is livingFor the molal quantity for being tested component；MMarkFor the molal quantity of internal standard compound；AIt is livingFor the corresponding signal of the feature structure The peak area at peak；AMarkFor the peak area at the internal standard compound characteristic signal peak of selection, fMarkFor unit molal quantity internal standard compound characteristic signal peak Peak area, fIt is livingThe peak area of the corresponding signal peak of component characteristics structure is tested for unit molal quantity.
7. a kind of method based on NMR technology fast quantification active Chinese drug component component according to claim 1, it is characterised in that: The dosage of the mixed solvent is 10~100 times for analyzing sample volume；The condition of the refrigerated centrifuge are as follows: centrifugal rotational speed is 500~4000rpm, sample room temperature be 20~60 DEG C, cryogenic temperature≤- 20 DEG C, the time be 2~for 24 hours.
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