CN111239315B - UPLC-DAD-MS-based analysis method for researching mailuoning injection fingerprint - Google Patents
UPLC-DAD-MS-based analysis method for researching mailuoning injection fingerprint Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
Abstract
The invention discloses an analysis method for researching a mailuoning injection fingerprint spectrum based on UPLC-DAD-MS, which is characterized in that on the basis of the research of early-stage chemical components, a mailuoning injection UPLC-DAD-MS liquid chromatography-mass spectrometry fingerprint spectrum is established, and 23 main components including 13 organic acids, 1 coumarin, 2 iridoids, 1 flavone, 1 lignan, 3 saponins and 2 other components can be directly analyzed and identified. The method can quickly obtain optimized chromatographic conditions, thereby obtaining the best fingerprint, having good reproducibility, accurately clarifying the main chemical composition of the Mailuoning injection, having important significance for clarifying the drug effect substance basis of the Mailuoning injection, and simultaneously laying a foundation for improving the quality control standard of the Mailuoning injection, establishing a scientific and reasonable quality control method and optimizing the preparation process.
Description
Technical Field
The invention relates to an analysis method for researching a mailuoning injection fingerprint spectrum based on UPLC-DAD-MS, belonging to the field of natural medicinal chemistry.
Background
Compared with the traditional dosage forms such as pills, powder, ointment, pills and the like, the traditional Chinese medicine injection is a novel traditional Chinese medicine dosage form with unique characteristics, and has the remarkable advantages that: the dosage is accurate, the medicine directly reaches the focus of a disease, the medicine has quick effect and reliable effect, and is a good choice for patients who are not suitable for oral administration or medicines which are not suitable for oral administration. The average growth rate of the traditional Chinese medicine injection market in China is over 30 percent in 1999-2009, more than 100 varieties of the traditional Chinese medicine injection exist in China, the average growth rate of the traditional Chinese medicine injection market in China is more than 30 percent, 3 hundred million patients use the traditional Chinese medicine injection every year, and the annual sales amount exceeds 150 hundred million yuan. However, the traditional Chinese medicine injection has a plurality of problems in the production and use processes, the quality standard is low, and the controllability is poor; the control means is lagged behind; the quality of the raw medicinal materials is not uniform; the most serious is unpredictability, diversity and multiplicity of adverse reactions brought by the traditional Chinese medicine injection after application, and sometimes serious consequences are brought, particularly, the injection varieties with adverse reactions clinically reported in recent years almost relate to all traditional Chinese medicine injections, the adverse reactions limit the development and application of the traditional Chinese medicine injections to a great extent, and the safety problem of the traditional Chinese medicine injections becomes one of the most concerned topics in the society.
The complexity of the ingredients of the traditional Chinese medicine preparation determines the diversity of the effects of the traditional Chinese medicine preparation, and before the effect is not clear, the effective ingredients, ineffective ingredients or toxic ingredients are difficult to distinguish, and perfect quality standards are difficult to establish for the effective ingredients, the ineffective ingredients or the toxic ingredients. In recent years, the country has increased the attention degree of traditional Chinese medicine, and in order to make the traditional Chinese medicine industry healthily develop, the country has successively issued a series of policy and regulations to standardize the research, declaration, production and use of traditional Chinese medicine injections. The basic technical requirements of traditional Chinese medicine and natural medicine injections issued by the State food and drug administration in 2007 put forward specific technical requirements on traditional Chinese medicine injections under research and development from aspects of non-clinical and clinical safety, medicine metabolism and the like, and put forward higher requirements on the basic research and quality standard of traditional Chinese medicine injections chemical substances. At present, the traditional Chinese medicine injection has the problems of unclear components, low quality control standard and great safety, so how to deeply research the traditional Chinese medicine injection by combining various advanced technologies makes the traditional Chinese medicine injection safer and more effective is a great challenge in front of the traditional Chinese medicine workers.
The Mailuoning injection is a compound Chinese medicine intravenous injection developed on the basis of clinical application of 'Simiaoyong' an decoction as one famous medical prescription, has independent intellectual property and is produced through scientific extraction and refining of Chinese medicinal materials including dendrobium stem, figwort, achyranthes root, honeysuckle and honeysuckle in 1985. The traditional Chinese medicine has the effects of promoting blood circulation to remove blood stasis, promoting qi circulation to relieve pain, nourishing yin to remove meridian obstruction and tonifying liver and kidney, is mainly used for treating diseases such as ischemic stroke acute stage, thromboangiitis obliterans, lower limb deep venous thrombosis, arteriosclerotic obliteration, cerebral infarction, angina, myocardial infarction, blood circulation disorder and sequelae thereof, has the total effective rate of 94.5 percent, has the advantages of quick response, high curative effect, short course of treatment, low price, less side effect, high safety and the like compared with similar medicines, becomes a nationwide special excellent Chinese patent medicine, and is widely applied in primary hospitals. In 1992, the Chinese medicine is listed as one of the first Chinese patent medicines which are necessary in emergency department of national institute of traditional Chinese medicine and the Chinese medicine protection variety; in 2000, 6 months, the Chinese patent medicine is listed as Chinese patent medicine A class medicine in the catalog of national basic medical insurance medicines; the 7-month-7-year-2009 selection of 307 new medical improvement basic drug catalogue versions in China is one of only 3 varieties of traditional Chinese medicine injections, and the medical improvement brings a new growth opportunity for the Mailuoning injection, is an excellent opportunity for a wider market, and shows strong vitality and a wide application prospect. According to incomplete statistics, the variety has been produced by 10 hundred million accumulated and the accumulated sales income is 100 hundred million yuan, thereby creating huge social and economic benefits.
The Mailuoning injection has wide clinical application and reliable curative effect, but the Mailuoning injection is a compound traditional Chinese medicine injection consisting of five medicinal materials, has interaction in the refining process, is never the simple addition of the medicinal materials, and has extremely complex components; the invention develops a series of innovative research works around a series of key scientific problems of quality reevaluation research of the Mailuoning injection, including substance basis separation, compound identification, effective substance content analysis and the like of the Mailuoning injection, aims to improve the content of detectable components in total solid in the Mailuoning and provides scientific basis for a series of research works of quality standard improvement, pharmacodynamic and pharmacokinetic research, production process optimization, adverse reaction source search and the like.
Disclosure of Invention
The invention relates to an analysis method for researching a mailining injection fingerprint based on UPLC-DAD-MS, which establishes a mailining injection UPLC-DAD-MS liquid chromatography-mass spectrometry fingerprint on the basis of the research of a former chemical component (patent 201910041593.9) and can directly analyze and identify 23 main components.
In order to achieve the purpose, the invention adopts the technical scheme that:
an analysis method for researching a mailuoning injection fingerprint spectrum based on UPLC-DAD-MS comprises the following analysis steps:
(1) Carrying out positive and negative ion full scanning by using UPLC-DAD-MS under a certain chromatographic mass spectrum condition to obtain a total ion flow diagram of the Mailuoning injection;
(2) The common peaks of the Mailuoning injection are determined to be 23 main components by fingerprint spectrum determination of more than three batches of Mailuoning injection and comparison with a reference substance through comparison of chromatograms, and the chemical structures are respectively as follows: dextroquinic acid, 5-hydroxymethylfurfural, protocatechuic acid, neochlorogenic acid, protocatechualdehyde, chlorogenic acid, cryptochlorogenic acid, 6,7-dihydroxycoumarin, caffeic acid, secoisolaricoside, p-hydroxycinnamic acid, secologenin, 1,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid (isochlorogenic acid A), luteolin, 3,4-dicaffeoylquinic acid (isochlorogenic acid B), syringaresinol, maillarin ester, caffeic acid ethyl ester, cinnamic acid, panax japonicus saponin 4A, alpha-hederagenin, and hederagenin-3-O-alpha-L-arabinopyranoside.
The UPLC-DAD-MS is 1260UPLC-DAD-6530ESI-QTOF MS produced by Agilent company of America; the chromatographic mass spectrum conditions are as follows: chromatographic column, agilent Zorbax SB-C 18 4.6mm × 100mm,1.8 μm,600bar; mobile phase a phase: 0.1% formic acid-water, phase B: methanol; the elution gradient is 0min 10% B,10min 20% B,20min 20% B,50min 50% B,70min100% B,85min 100% B; flow rate 0.3 mL/min -1 (ii) a The sample injection amount is 5 mu L; the column temperature is 35 ℃; DAD detection wavelength 254nm; mass spectrometer ESI ion source, negative ion mode (100-1700 m/z); atomizer pressure (Nebulizer pressure) 50psi; drying Gas Flow rate (Drying Gas Flow) 10 mL/min -1 (ii) a Drying Gas temperature (Drying Gas Temp) 350 ℃; capillary Voltage (Capillary Voltage) 3500V; fragmentor voltage 0-5min195V,5-60min135V,60-85min175V.
The reference substance is chlorogenic acid solution.
0.5mL of Mailuoning injection is diluted by adding 0.5mL of pure water to be used as a test solution.
Has the advantages that: the invention establishes a mailuoning injection UPLC-DAD-MS liquid chromatography-mass spectrometry fingerprint spectrum, and can directly analyze and identify 23 main components, including 13 organic acids, 1 coumarin, 2 iridoid, 1 flavone, 1 lignan, 3 saponins and 2 other components. The method can quickly obtain optimized chromatographic conditions, thereby obtaining the best fingerprint, having good reproducibility, accurately clarifying the main chemical composition of the Mailuoning injection, having important significance for clarifying the drug effect substance basis of the Mailuoning injection, and simultaneously laying a foundation for improving the quality control standard of the Mailuoning injection, establishing a scientific and reasonable quality control method and optimizing the preparation process.
Drawings
FIG. 1 is an enlarged view of ultraviolet fingerprint (254 nm) A0-35 min and B35-85 min of Mailuoning injection;
FIG. 2 is an enlarged view of Mailuoning injection total ion flow fingerprint spectrum C0-35 min and D35-85 min.
Detailed Description
Example 1
Instruments, reagents and samples
One in ten million electronic balance Mettler AE240; agilent 1260UPLC-DAD-6530ESI-QTOF MS; the device comprises the following components: G1322A,1260Degasser; G1312B,1260Bin Pump; G1367E,1260Hip ALS; G1316C,1290TCC; G4212B,1260DAD; G6530A,6530Accurate-Mass Q-TOF LC/MS; massHunter B0.05.0 workstation. Veillonning injection, nanjing Jinling pharmaceutical factory, jinling pharmaceutical industry, inc.; chlorogenic acid standard, china pharmaceutical biologicals institute, lot number 110753-201314 (content is 96.6%); methanol, merck (pesticide residue grade); formic acid, ruyi ROE in usa (> 99%, LCMS grade); deionized purified water (18 Ω).
Experimental methods
1. Preparation of test solution
1.1 chlorogenic acid Standard solution
Precisely weighing 10mg chlorogenic acid (content is 96.6%), placing in a 10mL volumetric flask, adding methanol to dissolve, and fixing volume to scale to 0.966 mg. ML -1 The chlorogenic acid mother liquor.
1.2 test article solution
Precisely sucking 0.5mL of Mailuoning injection, and adding 0.5mL of pure water for dilution.
2. Optimization of high performance liquid chromatography conditions the optimum chromatography conditions were determined by optimizing the chromatography conditions:
the instrument Agilent 1260UPLC-DAD-6530ESI-QTOF MS;
agilent Zorbax SB-C chromatographic column 18 4.6mm×100mm，1.8μm，600bar；
Mobile phase a phase: 0.1% formic acid-water, phase B: methanol;
elution gradient, 0min 10% B,10min 20% B,20min 20% B,50min 50% B,70min100% B,85min 100% B;
flow rate 0.3 mL/min -1 ；
The sample injection amount is 5 mu L;
the column temperature is 35 ℃;
DAD detection wavelength 254nm;
the test result shows that the separation degree of each spectrogram is good.
3. Optimization of mass spectrometry conditions
Data Acquisition and instrument parameter optimization are carried out by using MassHunter Data Acquisition software, qualitative Analysis is carried out by using quantitative Analysis software, and surfactants such as Tween and the like in the Mailuoning injection liquid are subjected to ion robbing in a positive ion mode, so that signals are disordered, and the response of each chemical component is good in a negative ion mode. Optimizing the Fragmentor voltage of the ESI ion source, wherein the size of the mass spectrum voltage influences a peak signal, the voltage is small, small molecular signals such as organic acid and the like are good, but large molecular component signals such as saponin and the like are weak; the voltage is high, small molecules such as organic acid and the like are broken, the signal is weak, but the saponin signal is strong, and certain influence is brought to quantitative detection.
Finally, determining mass spectrum conditions as follows:
mass spectrometer ESI ion source, negative ion mode (100-1700 m/z);
atomizer pressure (Nebulizer pressure) 50psi;
drying Gas Flow rate (Drying Gas Flow) 10 mL/min -1 ；
Drying Gas temperature (Drying Gas Temp) 350 ℃;
capillary Voltage (Capillary Voltage) 3500V;
fragmentor voltage 0-5min195V,5-60min135V,60-85min175V.
4. Determination of finger print
4.1 selection of reference substance because the ratio of the peak area of chlorogenic acid in the spectrum is large and stable, it was selected as reference substance (S).
4.2 fingerprint
Detecting by the above-mentioned determined chromatogram and mass spectrum method to obtain ultraviolet fingerprint (figure 1) and total ion flow fingerprint (figure 2).
4.3 determination of common peaks
Comparing the three batches of injection by fingerprint chromatogram determination and comparison with reference substances, and determining 23 common peaks by comparing chromatogram, wherein the ultraviolet fingerprint chromatogram can identify 17 peaks, and 6 peaks exceeding 5% of total peak area are No. 1 peak (D-quinic acid), no. 4 peak (neochlorogenic acid), no. 6 peak (peak chlorogenic acid), no. 7 peak (cryptochlorogenic acid), no. 9 peak (caffeic acid) and No. 12 peak (seco-loglycoside); wherein the total ion current fingerprint chromatogram can identify 23 peaks, and 5 chromatographic peaks exceeding 5% of the total peak area are No. 1 peak (D-quinic acid), no. 4 peak (neochlorogenic acid), no. 6 peak (peak chlorogenic acid), no. 9 peak (caffeic acid) and No. 12 peak (seco-loglycoside). The technical parameters are as follows: the relative retention times and peak area ratios of the common peaks are shown in Table 1.
TABLE 1 common Peak relative Retention time and Peak area ratio
5 methodology study
5.1 stability test
The same batch of sample solution (batch number 201204) is taken and subjected to sample injection measurement at 0,3,6, 12 and 24 hours respectively, and the result shows that (table 2), the RSD of the ratio of the relative peak areas of the common peak ratios in the fingerprint is less than 3%, which indicates that the sample is stable within 24 hours.
TABLE 2 stability results
5.2 repeatability test
Taking the same batch of sample solution (batch number 201204), preparing 6 parts of sample solution in total, respectively carrying out sample injection detection, calculating the ratio of all common peaks in the fingerprint, and obtaining a result (shown in table 3), wherein the RSD of the ratio of the relative peak areas is less than 5%, which indicates that the method has good repeatability.
TABLE 3 repeatability results
5.3 precision test
The same batch of sample solution (batch number 201204) is continuously injected for 6 times, the result can be seen (table 4), the common peak ratio of all common peaks in the fingerprint spectrum, and the RSD of the relative peak area ratio is less than 5%, which indicates that the method has good precision.
TABLE 4 results of precision
6 results and discussion
In order to determine the medicinal material source of each peak in the Mailuoning injection fingerprint, the literature search is carried out, and 19 peaks (No. 1-7,9-16, 19-20, 22-23) derived from honeysuckle medicinal materials are obtained; peaks derived from figwort include 2 (No. 9, 11); 1 peak from achyranthes bidentata (No. 23); peaks from shiga (No. 8, 11, 17, 20). Wherein, the No. 2 peak is generated by the hydrolysis of glucose and the like in the preparation, and the No. 18 peak is synthesized in the preparation process. The content of each peak was calculated from the control and the average of the multiple samples is shown in table 5.
TABLE 5 determination results of the content of main ingredients in Mailuoning injection
Claims (3)
1. An analysis method for researching a mailuoning injection fingerprint spectrum based on UPLC-DAD-MS is characterized by comprising the following analysis steps:
(1) Carrying out negative ion full scanning by using UPLC-DAD-MS under a certain chromatographic mass spectrum condition to obtain a total ion flow diagram of the Mailuoning injection;
(2) The common peaks are determined to be 23 main components by more than three batches of mailuoning injection fingerprint determination and comparison with a reference substance and comparison of chromatograms, and the chemical structures are respectively as follows: dextro-quinic acid, 5-hydroxymethylfurfural, protocatechuic acid, neochlorogenic acid, protocatechualdehyde, chlorogenic acid, cryptochlorogenic acid, 6,7-dihydroxycoumarin, caffeic acid, secoisolaricoside, p-hydroxycinnamic acid, secologenin, 1,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid (isochlorogenic acid A), galuteolin, 3,4-dicaffeoylquinic acid (isochlorogenic acid B), syringaresinol, mailuoning ester, caffeic acid ethyl ester, cinnamic acid, panax japonicus saponin 4A, alpha-hederagenin, hederagenin-3-O-alpha-L-arabinopyranoside;
the chromatographic mass spectrum conditions are as follows: chromatographic column, agilent Zorbax SB-C 18 4.6mm × 100mm,1.8 μm,600bar; mobile phase a phase: 0.1% formic acid-water, phase B: methanol; an elution gradient of 0min 10% B,10min 20% B,20min 20% B,50min 50% B,70min100% B,85 min100% B; flow rate 0.3 mL/min -1 (ii) a The sample injection amount is 5 mu L; the column temperature is 35 ℃;
the mass spectrum conditions are as follows: detector ESI ion source, negative ion mode 100-1700m/z; atomizer pressure 50psi; drying gasFlow rate 10 mL/min -1 (ii) a The temperature of the drying gas is 350 ℃; capillary voltage 3500V; fragment voltage 0-5min195V,5-60min135V,60-85min175V;
DAD detection wavelength 254nm; the reference substance is chlorogenic acid solution.
2. The method for analyzing the fingerprint of the research choroidning injection based on UPLC-DAD-MS as claimed in claim 1, wherein said UPLC-DAD-MS is 1260UPLC-DAD-6530ESI-QTOF MS manufactured by Agilent, USA.
3. The method for analyzing the fingerprint of the puling-based choroid ning injection based on UPLC-DAD-MS study of claim 1 wherein the puling-based injection is 0.5mL diluted with 0.5mL of purified water to obtain the test solution.
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| CN111638299A (en) * | 2020-07-06 | 2020-09-08 | 广西中医药大学 | Method for establishing Angelica keiskei high-performance liquid chromatography fingerprint |
| CN114166954B (en) * | 2021-04-07 | 2023-10-17 | 国药集团同济堂（贵州）制药有限公司 | Preparation method and quality detection method of black bone vine standard decoction |
| CN113607847A (en) * | 2021-08-03 | 2021-11-05 | 山东中医药大学 | Method for determining contents of various phenolic acid components in honeysuckle |
| CN113607848A (en) * | 2021-08-03 | 2021-11-05 | 山东中医药大学 | Method for simultaneously measuring multiple phenolic acids in honeysuckle |
| CN114166980A (en) * | 2021-12-28 | 2022-03-11 | 山西振东泰盛制药有限公司 | Method for constructing lignan fingerprint in ginkgo leaf medicinal material, extract and single preparation thereof |
| CN116242933A (en) * | 2023-01-17 | 2023-06-09 | 河北省药品医疗器械检验研究院(河北省化妆品检验研究中心) | Method for measuring content of 8 ingredients in Xiongju Shangqing tablet |
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| CN1304840C (en) * | 2004-03-16 | 2007-03-14 | 金陵药业股份有限公司 | Method for quality control of injections for treating thromboangitis diseases |
| CN1679648A (en) * | 2004-04-09 | 2005-10-12 | 北京奇源益德药物研究所 | Mailuoning injection and its preparation and quality control |
| CN100455315C (en) * | 2005-10-31 | 2009-01-28 | 石药集团欧意药业有限公司 | Injecting Mailuoning, its preparation and quality control thereof |
| CN101085224B (en) * | 2006-06-08 | 2011-11-30 | 天津天士力之骄药业有限公司 | Detection method of 'Mailuoning' injection preparation |
| CN101153866A (en) * | 2007-10-19 | 2008-04-02 | 中国药科大学 | Novel analysis method for complex composition of traditional Chinese medicine injection based on LC/MS-IT-TOF |
| CN109596751B (en) * | 2019-01-16 | 2021-07-06 | 金陵药业股份有限公司 | Mailuoning oral liquid component detection method for clearing heat, nourishing yin, promoting blood circulation and removing blood stasis |
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