CN104897840A - Novel method for quality control on polypeptide (oligopeptide) components in Shuxuetong injection - Google Patents
Novel method for quality control on polypeptide (oligopeptide) components in Shuxuetong injection Download PDFInfo
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- CN104897840A CN104897840A CN201510337719.9A CN201510337719A CN104897840A CN 104897840 A CN104897840 A CN 104897840A CN 201510337719 A CN201510337719 A CN 201510337719A CN 104897840 A CN104897840 A CN 104897840A
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Abstract
The invention relates to a quality control method of a traditional Chinese medicine preparation. Particularly, an HPLC (high performance liquid chromatography) is used for separation, an MS (mass spectrum) is used for detection, MRM (multiple reaction monitoring) is combined, an LC-MS-MRM separation, detection and statistical identification combined quality control model for a Shuxuetong injection is established, and the model is used for performing quality control on polypeptide (oligopeptide) components in the Shuxuetong injection. Qualitative identification can be performed on the known active polypeptide (oligopeptide) components in the Shuxuetong injection quickly and effectively with the method, and the method is simple, quick, high in specificity, good in reproducibility and more beneficial to improvement on a quality control means for the Shuxuetong injection.
Description
Technical field
The invention belongs to Analysis of Chinese Traditional Medicine field, relate to a kind of method of quality control of Chinese medicine preparation, specifically, a kind of liquid chromatography (HPLC) is adopted to be separated exactly, mass spectrum (MS) detects, in conjunction with multiple-reaction monitoring (MRM), the LC-MS-MRM setting up SHUXUETONG ZHUSHEYE is separated, detects, adds up the Quality Control Model identified and combine, and carries out the quality control of polypeptide (oligopeptides) constituents in SHUXUETONG ZHUSHEYE with this model.
Background technology
Traditional Chinese medicine and formulation chemist composition various and complicated, the diversity of its material base and complicacy just, jointly explain the wholistic therapy theory of traditional Chinese medicine and the material base of multiple target effect, in recent years, the carrying out that material foundation of tcm research is like a raging fire, but on a small quantity, there is the bottleneck broken through in trace and trace materials research aspect, under normal circumstances, these materials play the part of very important role in traditional Chinese medicine prevention and therapy disease, how to determine that in Chinese medicine and preparation thereof, these are a small amount of, trace and trace materials, and these materials are adopted simple, easy and method that is science carries out quality control, it is the difficult problem that traditional Chinese medicine practitioner needs to capture.
SHUXUETONG ZHUSHEYE is that friend fights national Chinese medicine two kind new medicine of medicine company independent research, extracted by leech, earthworm and refined and form, for domestic first animal compound liquid drugs injection formulation kind, there is promoting blood circulation and removing blood stasis, clearing and activating the channels and collaterals effect, be mainly used in the acute period of cerebral infarction caused by obstruction of collaterals by blood stasis, effectively can improve the symptoms such as the facial paralysis because cerebral ischemia causes, hemiplegia, dysphasia.The large constituents of SHUXUETONG ZHUSHEYE is mainly containing endogenous Small molecular base class, free amino acid, free monosaccharide, micromolecule polypeptide (oligopeptides), multiple large constituents such as oligosaccharides or glycopeptide, the micromolecule polypeptide (oligopeptides) that it has been generally acknowledged that in Shu Xue-tong may be the active component of Shu Xue-tong onset, but because content is very micro-, adopt HPLC direct injected and conventional detector analysis, be difficult to obtain good signal response, what the present SHUXUETONG ZHUSHEYE national drug standards adopted for the analysis of wherein polypeptide class component is amino acid derivedization HPLC analytic approach indirect determination before conventional post, mainly by the free aminoacid content in amino acid content deduction sample total after working sample hydrolysis, conversion polypeptide class component concentration wherein, process of the test is complicated, complex operation, if misoperation, interference and the not strong problem of specificity may be there is, and it is not characteristics strong to its real polypeptide (oligopeptides) class component.
MS-MRM (multiple reaction monitoring) technology is based on Given information or supposition information setting Mass Spectrometer Method rule, signal record is carried out to legal ion, remove the interference not meeting regular ion signal in a large number, thus obtain a kind of data acquiring mode of Information in Mass Spectra.Specifically, namely be according to polypeptide parent ion mass number and fragment ion masses number, select parent-daughter ion pair, the parent ion meeting setting is allowed to enter collision cell, after having collided, only record setting daughter ion signal, by twice selection of parent ion and daughter ion, remove interfering ion, reduce Chemical Background, improve sensitivity, MS-MRM analyzes can obtain the quantitative data with enough statistical significances, for selected parent ion-ion pair, mass spectrometer can adjust corresponding peptide section fragmentation energies, the mass spectrum response signal of effective raising fragmention, improve the sensitivity that peptide section detects, and can be implemented in the analysis of a mass spectrum sample introduction analysis reached hundreds of and even thousands of target peptide sections, improve detection efficiency, utilize MS-M R M technology specificity, the polypeptide meeting setting is detected, and carry out the analysis of enhancing Product scan further, obtain high-resolution tandem mass spectrum (MS/MS) crumb data, qualitative results false positive rate in analytic process is reduced greatly.Based on aforementioned techniques means, the present invention intends selecting suitable sample-pretreating method, the desalination of SHUXUETONG ZHUSHEYE is such as realized by means of molecular sieve column chromatography, and the enrichment that can realize interested polypeptide (oligopeptides) class component, by HPLC, polypeptide (oligopeptides) class component is wherein separated further again, by MRM technology, by MS detecting device, scanning analysis is carried out to the target peptide section parent ion and daughter ion that meet setting rule, eliminate interfering ion, reduce Chemical Background, improve sensitivity for analysis, thus establish the identification of means of polypeptide (oligopeptides) class component in a kind of SHUXUETONG ZHUSHEYE, identification and analysis can be carried out fast to related polypeptide (oligopeptides) the class component in SHUXUETONG ZHUSHEYE, thus the qualitative and quality control realized further polypeptide (oligopeptides) the class component in SHUXUETONG ZHUSHEYE.
Summary of the invention
1, goal of the invention
A kind of liquid chromatography (HPLC) is the object of the present invention is to provide to be separated, mass spectrum (MS) detects, in conjunction with multiple-reaction monitoring (MRM), the LC-MS-MRM setting up SHUXUETONG ZHUSHEYE is separated, detects, adds up the Quality Control Model identified and combine, and carries out the quality control of polypeptide (oligopeptides) constituents in SHUXUETONG ZHUSHEYE with this model.
2, concrete technical scheme of the present invention
In SHUXUETONG ZHUSHEYE polypeptide (oligopeptides) constituents detection method, comprise the steps:
(1) SHUXUETONG ZHUSHEYE need testing solution is carried out desalting processing
Desalination can adopt column chromatography or dialysis treatment, preferred molecular sieve column chromatography or ion-exchange chromatography desalting processing, further preferred molecular sieve column chromatography desalting processing.Molecular sieve column chromatography filler can be sephadex (sephadex G or sephacryl S) series, also can be polyacrylamide gel (BIO-Gel P) series, or Ago-Gel (Sepharose) series, preferred sephadex series sephadex G10, sephadex G15 or sephadex G25, further preferred sephadex G15 or sephadex G25 filler, eluant, eluent preferred water.
(2) HPLC is separated
By the desalted sample solution high speed centrifugation of collection or after crossing 0.2 μm of filter membrane, carry out HPLC separation.Common liquid phase chromatogram condition can be adopted to be separated, also can to carry out receiving rising liquid phase chromatogram condition analysis, also can adopt Ultra Performance Liquid Chromatography condition analysis.Further optimize common liquid phase chromatogram condition: chromatographic column adopts C18 to be Stationary liquid, and mobile phase A is 0.1% aqueous formic acid, and Mobile phase B is acetonitrile or 0.1% formic acid acetonitrile solution, and flow velocity and gradient condition can suitably adjust according to chromatographic column used.When select receive rise liquid chromatography time, preferable flow rate is 0.4 μ l/min, preferred gradient elution requirement: 0 ~ 6min, B are 5% → 8%; 6 ~ 40min, B are 8% → 30%; 40 ~ 45min, B are 30% → 60%; 45 ~ 48min, B are 60% → 80%; 48 ~ 56min, B are 80%; 56 ~ 58min, B are 80% → 5%; 58 ~ 65min, B are 5%.When selection UHPLC chromatographic column used, flow velocity is 0.1 ~ 0.3ml/min preferably, and condition of gradient elution is preferably: 0 ~ 2min, B are 5% → 8%; 2 ~ 13min, B are 8% → 30%; 13 ~ 15min, B are 30% → 60%; 15 ~ 16min, B are 60% → 80%; 16 ~ 18min, B are 80%; 18 ~ 19min, B are 80% → 5%; 19 ~ 22min, B are 5%.
(3) MS analyzes
The peptide class component be separated by HPLC, enters mass detector analysis successively.Its Mass Spectrometry Conditions optimized is: electric spray ion source (ESI), atomization gas and dry gas are nitrogen.Further be defined as gathering positive ion mode; One-level sweep limit: 350-2000Da; One-level scanning resolution: 70000; Secondary sweep limit: depend on one-level parent ion mass-to-charge ratio and automatically select; Secondary collision energy (NCEs): 28%; Secondary scanning resolution: 17500; Capillary temperature: 360 DEG C; Ion source voltage: 1800V; Fragmentation mode: HCD.
(4) MRM monitoring
Information in Mass Spectra according to target peptide section carries out qualitative analysis.By selecting multiple particular target peptide section component, preferably composition determines the polypeptide of molecular weight between 256-2560 dalton (oligopeptides) constituents further, further optimize composition and determine the polypeptide of molecular weight between 1000-2000 dalton (oligopeptides) constituents, carry out selecting the parent ion of peptide section and the monitoring of particular child ion, parent ion and particular child ion all should have good to mate and signal response is then thought and identified successfully with database.
3, beneficial effect of the present invention
The method is adopted to be conducive to, to SHUXUETONG ZHUSHEYE quality control, further ensureing product safety.About the mensuration of polypeptide in existing SHUXUETONG ZHUSHEYE quality standard, based on the own free ammonia amino acid of total amino acid deduction sample after hydrolysis, obtain the content of polypeptide class component, hydrolysis stage needs elevated-temperature seal, no matter and hydrolysis time is very long, usually need 24h, be that free amino acid or the mensuration of total amino acid all need pre-column derivatization, complex operation and unstable, also determines not to the sign of polypeptide fractions.And use analytical approach provided by the present invention, fast and effeciently can carry out Qualitative Identification to known activity polypeptide (oligopeptides) component in SHUXUETONG ZHUSHEYE, the analytical approach that simultaneously the present invention sets up have method simple, fast, strong, the high repeatability and other advantages of specificity, be more conducive to the quality control method promoting Shu Xue-tong note parenteral solution further.
Accompanying drawing explanation
Fig. 1: polypeptide YB-001 chooses particular child ion fragment chromatogram
Fig. 2: polypeptide YB-001 chooses daughter ion fragments mass spectrogram and database matching collection of illustrative plates
Fig. 3: polypeptide YB-002 chooses particular child ion fragment chromatogram
Fig. 4: polypeptide YB-002 chooses daughter ion fragments mass spectrogram and database matching collection of illustrative plates
Fig. 5: polypeptide YB-003 chooses particular child ion fragment chromatogram
Fig. 6: polypeptide YB-003 chooses daughter ion fragments mass spectrogram and database matching collection of illustrative plates
Embodiment
For feature of the present invention, technological means and the specific purposes reached, function can be understood further, resolve the advantages and spirit of the present invention, further illustrate the present invention below by way of specific embodiment, but be not construed as limiting the invention.
Embodiment:
Instrument: HPLC model: Eksigent 425nano LC; MS model: AB SCIEX
6500;
Shu Xue-tong sample: Mudanjiang Youbo Pharmaceutical Co., Ltd. produces.
Sample preparation: get SHUXUETONG ZHUSHEYE 1ml, in careful loading to the good Sephadex G15 chromatographic column of pre-balance (chromatographic column specification: 1.4cm*8cm), with deionized water wash-out and Fractional Collections water elution liquid, uses 0.1M AgNO
3detect to occurring that namely white opacity stops collecting, the water elution liquid collected before merging.As need testing solution, carry out LC-MS-MRM analysis.
Chromatographiccondition: self-control nozzle needle one scapus, 75 μm × 15cm, filler is: Venusil × BP, C18 (L), 5 μm,
(Ai Jieer Agela Technologies company), flow velocity is 0.4 μ l/min, and mobile phase A is 0.1% aqueous formic acid, and Mobile phase B is 0.1% formic acid acetonitrile solution, and condition of gradient elution is as follows: 0 ~ 6min, B:5% → 8%; 6 ~ 40min, B:8% → 30%; 40 ~ 45min, B:30% → 60%; 45 ~ 48min, B:60% → 80%; 48 ~ 56min, B:80%; 56 ~ 58min, B:80% → 5%; 58 ~ 65min, B:5%;
Mass spectrophotometry condition: adopt electric spray ion source (ESI), atomization gas and dry gas are nitrogen; MRM is taked to scan.Gather ion mode: positive ion mode; One-level sweep limit: 350-2000Da; One-level scanning resolution: 70000; Secondary sweep limit: depend on one-level parent ion mass-to-charge ratio and automatically select; Secondary collision energy (NCEs): 28%; Secondary scanning resolution: 17500; Capillary temperature: 360 DEG C; Ion source voltage: 1800V; Fragmentation mode: HCD.
Analysis software: SKYLINE software
Analytical approach: extract the target peptide section 3 (polypeptide YB-001 ~ YB-003) meeting MRM standard with SKYLINE software, select suitable transition to carry out MRM detection.
Analysis and Identification result: by peptide section parent ion and the Information in Mass Spectra comparison choosing daughter ion, detect 3 target peptide sections, and all have reasonable signal response, good with associated mass spectrometry Data Matching in database, can assert in SHUXUETONG ZHUSHEYE containing corresponding 3 target peptide section components (accompanying drawing 1 ~ accompanying drawing 6).
Claims (7)
1. a new method for polypeptide (oligopeptides) constituents quality control in SHUXUETONG ZHUSHEYE, it is characterized in that, the method comprises the steps:
(1) SHUXUETONG ZHUSHEYE is carried out the pre-treatments such as desalination; (2) desalted sample solution is carried out high performance liquid chromatography (HPLC) to be separated; (3) sample that liquid chromatography is separated is carried out mass spectrum (MS) analysis; (4) adopt multiple-reaction monitoring pattern (MRM), the Information in Mass Spectra according to target peptide section carries out qualitative analysis.
2. method according to claim 1, it is characterized in that, wherein in step (1), the desalination of SHUXUETONG ZHUSHEYE adopts column chromatography or dialysis treatment, preferred molecular sieve column chromatography or ion-exchange chromatography desalting processing, further preferred molecular sieve column chromatography desalting processing.
3. molecular sieve column chromatography desalting processing method according to claim 2, molecular sieve column chromatography filler can be sephadex (sephadex G or sephacryl S) series, also can be polyacrylamide gel (BIO-Gel P) series, or Ago-Gel (Sepharose) series, preferred sephadex series sephadex G10, sephadex G15 or sephadex G25, further preferred sephadex G15 or sephadex G25 filler, eluant, eluent preferred water.
4. method according to claim 1, it is characterized in that, the liquid chromatography wherein described in step (2) is separated, and common liquid phase chromatogram condition can be adopted to be separated, also can carry out receiving rising liquid phase chromatogram condition analysis, also can adopt Ultra Performance Liquid Chromatography condition analysis.Further optimize common liquid phase chromatogram condition: chromatographic column adopts C18 to be Stationary liquid, and mobile phase A is 0.1% aqueous formic acid, and Mobile phase B is acetonitrile or 0.1% formic acid acetonitrile solution, and flow velocity and gradient condition can suitably adjust according to chromatographic column used.When select receive rise liquid chromatography time, preferable flow rate is 0.4 μ l/min, preferred gradient elution requirement: 0 ~ 6min, B are 5% → 8%; 6 ~ 40min, B are 8% → 30%; 40 ~ 45min, B are 30% → 60%; 45 ~ 48min, B are 60% → 80%; 48 ~ 56min, B are 80%; 56 ~ 58min, B are 80% → 5%; 58 ~ 65min, B are 5%.When selection UHPLC chromatographic column used, flow velocity is 0.1 ~ 0.3ml/min preferably, and condition of gradient elution is preferably: 0 ~ 2min, B are 5% → 8%; 2 ~ 13min, B are 8% → 30%; 13 ~ 15min, B are 30% → 60%; 15 ~ 16min, B are 60% → 80%; 16 ~ 18min, B are 80%; 18 ~ 19min, B are 80% → 5%; 19 ~ 22min, B are 5%.
5. method according to claim 1, it is characterized in that, wherein described in step (3) by liquid chromatography be separated sample carry out mass spectrophotometry, its optimize Mass Spectrometry Conditions: electric spray ion source (ESI), atomization gas and dry gas are nitrogen.Further be defined as gathering positive ion mode; One-level sweep limit: 350-2000Da; One-level scanning resolution: 70000; Secondary sweep limit: depend on one-level parent ion mass-to-charge ratio and automatically select; Secondary collision energy (NCEs): 28%; Secondary scanning resolution: 17500; Capillary temperature: 360 DEG C; Ion source voltage: 1800V; Fragmentation mode: HCD.
6. method according to claim 1, it is characterized in that, employing multiple-reaction monitoring pattern (MRM) wherein described in step (3), Information in Mass Spectra according to target peptide section carries out qualitative analysis, specifically, select multiple particular target peptide section component exactly, carry out the monitoring of specific parent ion and daughter ion, parent ion and particular child ion all should have with database and mate preferably and signal response is then thought and identified successfully.
7. the particular target peptide section component selected in multiple-reaction monitoring pattern (MRM) according to claim 6, specifically refer to related polypeptide (oligopeptides) the class component in SHUXUETONG ZHUSHEYE, preferably composition determines the polypeptide of molecular weight between 256-2560 dalton (oligopeptides) constituents further, further optimizes composition and determines the polypeptide of molecular weight between 1000-2000 dalton (oligopeptides) constituents.
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| CN112557527A (en) * | 2020-11-17 | 2021-03-26 | 牡丹江友搏药业有限责任公司 | Method for measuring polypeptide content in Shuxuetong injection |
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