CN104849382A - Rapid analysis method of unknown sesquiterpenes pyridine alkaloids in thunder god vine - Google Patents
Rapid analysis method of unknown sesquiterpenes pyridine alkaloids in thunder god vine Download PDFInfo
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Abstract
The invention relates to a rapid mass spectrometry method for indentifying unknown sesquiterpenes pyridine alkaloids in thunder god vine, which belongs to the pharmacy field. The method comprises the following steps: processing Chinese fevervine herb by a pre-treatment process of a sample through solvent ultrasonic extraction; using an electro-spray, a quadrupole and a time-of-flight mass spectrometer for analyzing fragment ions of the known single sesquiterpenes pyridine alkaloid, especially analyzing the fragment ions through frame cracking; using a high performance liquid chromatography, the electro-spray and the quadrupole and the time-of-flight mass spectrometer to obtain a secondary mass spectrum of sesquiterpenes pyridine alkaloids in a complex system to obtain the fragment ions of an unknown compound, wherein a profile diagram of the fragment ions of sesquiterpenes pyridine alkaloid in the complex system can be respectively obtained by using two methods; comparing the profile diagram of the fragment ions of the sesquiterpenes pyridine alkaloid in the known complex system and the complex system and comparing the characteristic fragment ions, and performing a rapid structural analysis on the unknown sesquiterpenes pyridine alkaloid in the complex system.
Description
Technical field
The invention belongs to medical art, relate to independent, the express-analysis of sesquiterpenes pyridine alkaloids composition unknown in thunder godvine.
Background technology
Thunder godvine (Tripterygium wilfordii Hook.f.) is Celastraceae tripterygium plant, is mainly distributed in southern china, is a kind of important traditional Chinese medicine material.Be used for the treatment of the autoimmune diseases such as rheumatoid arthritis, chronic nephritis, erythema wolf storehouse, contact dermatitis, all have conspicuousness curative effect.
Sesquiterpenes pyridine alkaloids is the very important active component of a class in tripterygium plant, and research shows that this compounds has anti-immunity, desinsection, anti-HIV (J.Nat.Prod.2000,63,357), anticancer isoreactivity.Therefore, numerous scientists has been attracted to study.The research of efficient analytical approach to biological field is most important, because biological field often relates to trace analysis.Analysis main is at present nuclear magnetic resonance, but nuclear-magnetism qualification needs to obtain sterling, therefore cannot realize carrying out express-analysis to the sesquiterpenes pyridine alkaloids of the relatively very low the unknown of content in thunder godvine.LC-MS technology is the method for unknown trace materials in a kind of important Analysis of Complex system, and current method often needs database (J.Am.Chem.Soc.2009,131,5030; Anal.Chem.2008,80,1280), but the database of LC-MS is very limited, and between different instruments, the reappearance of second order ms is poor, and in addition, the standard natural products obtaining trace is very difficult; The difficulty that numerous isomerss adds analysis is there is in plant.Therefore, need to set up a kind of practicality, analytical approach is for the express-analysis of sesquiterpenes pyridine alkaloids unknown in thunder godvine fast.
Summary of the invention
The object of this invention is to provide that a kind of mass spectrometry method is for the express-analysis of sesquiterpenes pyridine alkaloids unknown in thunder godvine reliably, fast.This method, in conjunction with liquid chromatography isolation technics, utilizes two kinds of methods to obtain compound second order ms figure in extracts, is analyzed by the profile diagram of second order ms in conjunction with the sesquiterpenes pyridine alkaloids compound of the characteristic ion in second order ms to the unknown.
Therefore, the analytical approach of unknown in thunder godvine provided by the invention sesquiterpenes pyridine alkaloids comprises the steps: that in (1) thunder godvine, active component extracts; (2) electron spray-fragmention of level Four bar-time of-flight mass spectrometer to known single sesquiterpenes pyridine alkaloids is utilized to analyze; (3) LC-MS analysis, namely utilizes high performance liquid chromatography-electron spray-level Four bar-time of-flight mass spectrometer to obtain the second order ms of sesquiterpenes pyridine alkaloids in complex system, namely obtains the fragmention of unknown compound; (4) by comparing the profile diagram of known compound and sesquiterpenes pyridine alkaloids fragmention in complex system and comparing their fragments characteristic ion, thus realize carrying out structure analysis analysis fast to sesquiterpenes pyridine alkaloids unknown in complex system.
Particularly, the analytical approach of unknown in thunder godvine provided by the invention sesquiterpenes pyridine alkaloids comprises the steps:
(1). the extraction of active ingredients of thunder god vine
Carry out ultrasonic lixiviate targetedly to the active component in thunder godvine, wherein lixiviate solubilising reagent is both mixed solvent any of water, methyl alcohol, second cyanogen, acetone, chloroform or above-mentioned solvent, and ultrasonic time is 1-5 hour, then filters.The inventive method leaching process should obtain many active components as far as possible, removes the interference of other composition such as pigment, sugar etc. again as far as possible.
(2). the fragmention analysis of known single sesquiterpenes pyridine alkaloids
Utilize the electron spray-fragmention of level Four bar-time of-flight mass spectrometer to known 14 kinds of single sesquiterpenes pyridine alkaloids to analyze (table one), the profile according to the design feature of these 14 kinds of compounds, cracking mode and secondary spectrogram is divided into 7 types.Cracking mode mainly contains side chain fracture, framework collapse, and sums up reaction between fragment.The side chain be wherein connected with C-1 easily adds and reacts, and the side chain be connected with C-2 is easily lost.
(3). LC-MS analysis
High performance liquid chromatography is utilized to be separated the potpourri obtained in step (1), select C18 post, corresponding separation condition (comprising the length of chromatographic column, internal diameter, filler, flow velocity, mobile phase composition, gradient, different electrolyte), Mass Spectrometry Conditions (parameter of instrument) are optimized by collection of illustrative plates.Application liquid chromatography-electron spray-level Four bar-time of-flight mass spectrometer carries out full scan analysis (wherein electron spray-level Four bar-flight time mass spectrum is a complete equipment, can be used for the spectrogram obtaining one-level and second order ms) in the positive-ion mode.Utilize two kinds of method choice impact energies to obtain fragmention profile diagram, wherein utilize respectively constant with impact energy that is gradient to obtain the profile diagram of fragmention, wherein the impact energy of gradient is directly proportional to the molecular weight of compound.
(4). the structure analysis of sesquiterpenes pyridine alkaloids in triperygium wilfordii extractive
By more known profile diagram with sesquiterpenes pyridine alkaloids fragmention in complex system and the fragments characteristic ion comparing them, differentiate dissimilar unknown sesquiterpenes pyridine alkaloids compound, it comprises: wherein fragmention m/z 206 in spectrogram, 204, or 194 is characteristic ions of pyridine moiety; Wherein m/z 310 is that two fragmentions sum up reaction generation, and this ion is relevant to side chain positions, can be used for identifying side chain positions; Other fragmention mainly comes from side chain and loses; Compound molecular weight, when more than 800Da, selects constant energy approach to be more suitable for for the identification of unknown compound, and compound molecular weight, when below 800Da, selects gradient energy method to be more suitable for for the identification of unknown compound.
The present invention has the following advantages:
1. can complete rapidly, independently sesquiterpenes pyridine alkaloids composition in thunder godvine, comprise the Structural Identification of unknown compound, do not need the analysis means in conjunction with other.
2. can complete the analysis to sesquiterpenes pyridine alkaloids composition in thunder godvine rapidly, independently, comprise the determination of some side chain positions.
3. the selection of two impact energies had both improve the confidence level of qualification, turn avoid the loaded down with trivial details of data, can be used for high throughput analysis.
Accompanying drawing explanation
Table one is the fragmention mass spectrophotometry (impact energy: 25eV) of known single sesquiterpenes pyridine alkaloids.
Figure mono-is the second order spectrum of (a) known compound cangorinine E-1, and the second order spectrum of compd A is known in the second order spectrum of (b) known compound wilforine and (c) the unknown;
Figure bis-is second order spectrums of (a) known compound euonymine, and the second order spectrum (impact energy is 25eV) of compd B is known in the second order spectrum (impact energy is 21eV) of (b) unknown compound B and (c) the unknown.
Embodiment
The present invention is explained below in conjunction with embodiment.Embodiment for ease of better understanding the present invention, but is not limitation of the present invention.
Embodiment 1:
(1). active ingredients of thunder god vine extracts
Thunder godvine is purchased from lotus pond market, Chengdu, and the ultrasonic immersion of 100% methyl alcohol low pressure thickening filtration after a hour, obtains corresponding solid.
(2). the fragmention of known single sesquiterpenes pyridine alkaloids is analyzed
Instrument: Brooker company ESI-Q-TOF (micrOTOF Q)
Mass Spectrometry Conditions: ionization mode, positive ion mode (+); Spray pressure power, 30psi; Argon gas is collision gas, impact energy, 25eV; Dry gas temperature, 180 DEG C; Kapillary port voltage ,-4500V, crown cap voltage ,-4000V.
The second order spectrum of known compound cangorinine E-1 is analyzed (accompanying drawing one (a)), research finds that the fragmention in high-quality district is lost mainly through fracture side chain, the fragmention of low mass region, the such as characteristic ion of m/z 206 mainly pyridine moiety, the fragmention m/z310 of feature is by adding and reacting formation.Although known compound wilforine and cangorinine E-1 is isomers, structure is also quite similar, but the profile diagram of their secondary spectrograms not identical (accompanying drawing one (b)), the more important thing is not have characteristic fragmention m/z310 in the secondary spectrogram of compound wilforine, this illustrates that the formation of this ion is relevant to the position of substitution of benzoic acid side chain.
(3). LC-MS is analyzed crude extract
Instrument: Brooker company HPLC-ESI-Q-TOF (micrOTOF Q)
Chromatographic condition: Agilent C18 chromatographic column (4.6 × 150,3.5 μm); Sample size: 10 μ l; Flow velocity: 1.0ml/min; Mobile phase forms: water (A) and second cyanogen (B); Gradient elution, 0-5min:35% (B), 5-55min:35-80% (B).
Mass Spectrometry Conditions: ionization mode, positive ion mode (+); Spray pressure power, 30psi; Dry gas temperature, 180 DEG C; Kapillary port voltage ,-4500V, crown cap voltage ,-4000V.Argon gas is collision gas, impact energy, 25eV.
Be we obtain the second order spectrum of unknown compound in complex system by LC-MS method, accompanying drawing one (c) provides the second order spectrum of unknown compound A.
(4). the structure analysis of sesquiterpenes pyridine alkaloids in triperygium wilfordii extractive
By the profile diagram of the second order spectrum of contrast unknown compound A and the second order spectrum of known compound cangorinine E-1, can determine that unknown compound A is identical with the skeleton of known compound cangorinine E-1.Further analysis finds, the ion of their low mass region is identical, therefore, pyridine moiety structure is identical, the fragmention m/z310 of feature can detect, illustrate that the position of benzoic acid side chain substituents is also identical, lose the molecular formula with them than the neutrality in better quality district, can determine that the structure of unknown compound A is as shown in figure mono-(c).
Embodiment 2:
(1). active ingredients of thunder god vine extracts
Thunder godvine is purchased from lotus pond market, Chengdu, and the ultrasonic immersion of 100% methyl alcohol low pressure thickening filtration after a hour, obtains corresponding solid.
(2). the fragmention of known single sesquiterpenes pyridine alkaloids is analyzed
Instrument: Brooker company ESI-Q-TOF (micrOTOF Q)
Mass Spectrometry Conditions: ionization mode, positive ion mode (+); Spray pressure power, 30psi; Argon gas is collision gas, impact energy, 25eV; Dry gas temperature, 180 DEG C; Kapillary port voltage ,-4500V, crown cap voltage ,-4000V.
The second order spectrum of known compound euonymine is analyzed (accompanying drawing two (a)), research finds that the fragmention in high-quality district is lost mainly through fracture side chain, the characteristic ion of the fragmention of low mass region mainly pyridine moiety.
(3). LC-MS is analyzed crude extract
Instrument: Brooker company HPLC-ESI-Q-TOF (micrOTOF Q)
Chromatographic condition: Féraud door C18 chromatographic column (4.6 × 150,3.5 μm); Sample size: 10 μ l; Flow velocity: 1.0ml/min; Mobile phase forms: water (A) and second cyanogen (B); Gradient elution, 0-5min:35% (B), 5-55min:35-80% (B).
Mass Spectrometry Conditions: ionization mode, positive ion mode (+); Spray pressure power, 30psi; Dry gas temperature, 180 DEG C; Kapillary port voltage ,-4500V, crown cap voltage ,-4000V.Argon gas is collision gas, impact energy, and a method is set to 25eV, and the collision of another method increases along with the increase of compound molecular weight.
(4). the structure analysis of sesquiterpenes pyridine alkaloids in triperygium wilfordii extractive
It is the second order spectrum of unknown compound B in triperygium wilfordii extractive in accompanying drawing two (b) and (c), wherein accompanying drawing two (b) is obtain under the condition of 21eV in impact energy, and accompanying drawing two (c) obtains under impact energy is the condition of 25eV.By comparative drawings figs two (a), (b) and (c), can determine to select impact energy to be the qualification that figure under the condition of 21eV is more suitable for unknown compound, profile diagram under this condition is more consistent with the profile diagram of known compound, and under constant energy condition, the profile diagram of collection of illustrative plates and the second order spectrum of known compound euonymine differ far away.
Table one. the fragmention mass spectrophotometry (impact energy: 25eV) of known single sesquiterpenes pyridine alkaloids.
Claims (5)
1. a rapid analysis for sesquiterpenes pyridine alkaloids unknown in thunder godvine, is characterized in that, in the method comprises (1) thunder godvine, active component extracts; (2) utilize the electron spray-fragmention of level Four bar-time of-flight mass spectrometer to known single sesquiterpenes pyridine alkaloids to analyze, particularly the fragmention coming from skeleton cracking is analyzed; (3) LC-MS analysis, namely high performance liquid chromatography-electron spray-level Four bar-time of-flight mass spectrometer is utilized to obtain the second order ms of sesquiterpenes pyridine alkaloids in complex system, namely obtain the fragmention of unknown compound, wherein make use of the profile diagram that two kinds of methods obtain sesquiterpenes pyridine alkaloids fragmention in complex system respectively; (4) by more known profile diagram with sesquiterpenes pyridine alkaloids fragmention in complex system and the fragments characteristic ion comparing them, thus realize carrying out skeleton and the analysis of C1 and C2 side-chain structure fast to sesquiterpenes pyridine alkaloids unknown in complex system.
2. the rapid analysis of sesquiterpenes pyridine alkaloids unknown in thunder godvine as claimed in claim 1, it is characterized in that, sesquiterpenes pyridine alkaloids unknown in thunder godvine wherein described in step (1) is extracted as ultrasonic lixiviate, wherein lixiviate solubilising reagent is both mixed solvent any of water, methyl alcohol, second cyanogen, acetone, chloroform or above-mentioned solvent, ultrasonic time is 1-5 hour, then filters.
3. sesquiterpenes pyridine alkaloids rapid analysis unknown in thunder godvine as claimed in claim 1 or 2, it is characterized in that, electron spray-the fragmention of level Four bar-time of-flight mass spectrometer to known single sesquiterpenes pyridine alkaloids that utilize wherein described in step (2) is analyzed, wherein the fragmention of sesquiterpenes pyridine alkaloids has and comes from side chain fracture in step (2), have and come from framework collapse, have and come from the generation that sums up reaction between fragment.
4. as claim 1, sesquiterpenes pyridine alkaloids rapid analysis unknown in thunder godvine described in 2 or 3, it is characterized in that, high performance liquid chromatography wherein described in step (3) is separated the potpourri obtained in step (1), select C18 post, column length 50-300mm, internal diameter 1-5mm, filler granularity 1.0-5.0 μm; Column temperature 15-60 DEG C; Sample size 2-50 μ l; Flow velocity 0.01-1ml/min; Mobile phase is made up of water, methyl alcohol or second cyanogen, increases formic acid, acetic acid, trifluoracetic acid, ammoniacal liquor, ammonium acetate or ammonium chloride in mobile phase, and its concentration is 0.01%-10%; Carry out gradient or isocratic elution; The sweep velocity of electron spray-level Four bar-time of-flight mass spectrometer is 50-0.1Hz; The window of Selective ion mode is 1-20u; Resolution is set to 10000-20000; Utilize positive ion mode analysis, capillary voltage is 4000-4500V; Two kinds of methods described in step (3) refer to utilize respectively constant with impact energy that is gradient to obtain the profile diagram of fragmention, wherein the impact energy of gradient is directly proportional to the molecular weight of compound.
5. as claim 1,2, sesquiterpenes pyridine alkaloids rapid analysis unknown in thunder godvine described in 3 or 4, it is characterized in that, wherein described in step (4) by more known profile diagram with sesquiterpenes pyridine alkaloids fragmention in complex system and the fragments characteristic ion comparing them, differentiate dissimilar unknown sesquiterpenes pyridine alkaloids compound, it comprises: wherein fragmention m/z 206 in spectrogram, 204, or 194 is characteristic ions of pyridine moiety; Wherein m/z 310 is that two fragmentions sum up reaction generation, and this ion is relevant to side chain positions, can be used for identifying side chain positions; Other fragmention mainly comes from side chain and loses; Compound molecular weight, when more than 800Da, selects constant energy approach to be more suitable for for the identification of unknown compound, and compound molecular weight, when below 800Da, selects gradient energy method to be more suitable for for the identification of unknown compound.
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Application publication date: 20150819 |