CN117686622A - Analysis method of multiple components in eight-ingredient zichongkusan - Google Patents
Analysis method of multiple components in eight-ingredient zichongkusan Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical component analysis, and provides a method for analyzing multiple components in eight-ingredient zichosla powder, which comprises the following steps: s1, preparing a sample solution: extracting the active ingredients of the eight-ingredient zichongsan sample with methanol solution, wherein the ratio of feed to liquid is 0.2g:5ml, centrifuging the extracting solution to obtain supernatant, and passing through a membrane to obtain a sample solution; s2, detecting and analyzing the sample solution by adopting a triple quadrupole time-of-flight high-resolution mass spectrum; s3, analyzing the data acquired by the mass spectrum, so as to analyze and identify the components of the eight-ingredient Chinese mosla herb powder. The invention adopts UPLC-Q-TOF-MS method to analyze and identify the chemical components of the eight-ingredient Qolsla powder, and provides basis for further researching the basic research of the drug effect substances of the eight-ingredient Qolsla powder.
Description
Technical Field
The invention relates to the technical field of chemical component analysis, in particular to a method for analyzing multiple components in eight-ingredient zichosla powder.
Background
Tibetan medicine is an important component of traditional Chinese medicine, and is attracting attention due to its unique medicine and medicine source. The Tibetan medicine has wide application range, and the curative effect is widely accepted and applied in clinical practice. The eight ingredients of the Chinese mosla herb powder is one of Tibetan medicines and is the result of the theory of the counterpart agent of the traditional Chinese medicine and the clinical application thereof. The Chinese medicinal composition comprises eight medicines of elsholtzia day, kombucha, allium sinense, tibetan rue, ash vegetable, radix angelicae pubescentis and artificial musk; has effects of dispelling pathogenic wind, removing dampness, sterilizing, relieving itching, clearing heat and toxic materials, dispelling cold, relieving swelling, relieving rigidity of muscles, activating collaterals, activating qi-flowing, relieving pain, and removing dampness and heat, and can be used for treating gynecological diseases, perianal inflammation, hemorrhoid, etc. Wherein, the herba Moslae Sibiricae has the effects of preventing insect and treating anus inflammation, and can be used for treating damp stagnation, distention, anorexia, abdominal pain, vomiting and diarrhea, insect accumulation, scabies, tinea, itching, and trichomonas vaginalis. The Chinese gooseberry is used for killing parasites, promoting stomach temperature, and mainly treating taeniasis and edema. The medicine recorded in the manna herbal open mirror records that the rabdosia amethystoides have the effects of diminishing inflammation, relieving pain and killing parasites and are mainly used for treating eye diseases such as trachoma, conjunctivitis and the like and gastrointestinal angina caused by parasites; the effect of the drooping fruit and allium sativum is detumescence, and is used for treating breast swelling and anthrax.
At present, pharmacological and pharmacodynamics researches of the eight-ingredient Chinese mosla herb powder are temporarily in a blank stage, only small-area and small-scale clinical medicine researches are performed, and no specific pharmacodynamics research is performed. However, it is particularly important and urgent to conduct specific pharmacodynamic studies on such prescriptions which are clinically used in a large number of Tibetan medicine and have good effects. Therefore, the main chemical components of the eight-ingredient zichosla powder are further explored, and the elucidation and the research on the action mechanism of the drug effect substances are very important.
Disclosure of Invention
The invention aims at: aiming at the problems, the invention provides a multi-component analysis method in the eight-ingredient Chinese mosla herb powder, which adopts triple quadrupole time-of-flight high-resolution mass spectrometry (UPLC-Q-TOF-MS) to analyze and identify chemical components in the eight-ingredient Chinese mosla herb powder, thereby providing basis for further researching the basic research of the drug effect substances of the eight-ingredient Chinese mosla herb powder.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the method for analyzing the multiple components in the eight-ingredient zichongkusan comprises the following steps:
s1, preparing a sample solution: taking an eight-ingredient Chinese mosla herb powder sample, extracting active ingredients of the eight-ingredient Chinese mosla herb powder sample by using a methanol solution, wherein the ratio of feed liquid to extract is 0.2g:5ml, centrifuging the extracting solution to obtain supernatant, and passing through a membrane to obtain a sample solution;
s2, detecting and analyzing the sample solution by adopting a triple quadrupole time-of-flight high-resolution mass spectrum, wherein the detection conditions comprise:
chromatographic conditions: the chromatographic column is C18, the specification is 2.1mm multiplied by 100mm, and the specification is 1.7 mu m; the column temperature is 45 ℃; the flow rate is 0.4ml/min; the sample injection amount is 4 μl; the mobile phase adopts a gradient elution program of acetonitrile-0.1% formic acid aqueous solution, and specifically comprises the following steps: 0-0.01 min,5% B; 0.01-15 min, 5-30% B; 15-35 min, 30-95% B; 35-37 min,95% B; 37-37.1 min, 95-5% B; 37.1-40 min, 5-0B; the concentrations are all volume percentages;
mass spectrometry conditions: the primary mass spectrum scanning is carried out, wherein the ionization mode is an electrospray positive ion mode, the ion source voltage is 5500V, the ion source temperature is 500 ℃, the declustering voltage is 100V, the collision energy is 35eV, and the collision energy is expanded to 15eV; the atomization gas is nitrogen, the auxiliary gas 1 is 50PSI, the auxiliary gas 2 is 50PSI, and the gas curtain gas is 40PSI; the scanning range of the primary mass spectrum parent ion is 50-1000, and the IDA sets 6 highest peaks with response values exceeding 100cps for secondary mass spectrum scanning; the scanning range of the sub-ions is 50-1000, dynamic background subtraction DBS is started, the ionization mode is an electrospray negative ion mode, the ion source voltage is-4500V, the ion source temperature is 500 ℃, the cluster removal voltage is 100V, the collision energy is-35 eV, and the collision energy is expanded to 15eV; the atomization gas is nitrogen, the auxiliary gas 1 is 50PSI, the auxiliary gas 2 is 50PSI, and the gas curtain gas is 40PSI;
s3, analyzing the data acquired by the mass spectrum, so as to analyze and identify the components of the eight-ingredient Chinese mosla herb powder.
In the present invention, preferably, the extraction is performed in step S1 using a methanol solution having a volume concentration of 50%.
In the present invention, preferably, the extraction is performed in the ultrasonic extraction manner in the step S1, and the extraction time is 45 minutes.
In the present invention, it is preferable that the centrifugation in step S1 is centrifugation at 13000rpm for 10min.
In the present invention, preferably, the analytical identification method in step S3 is as follows: first, referring to the literature to obtain data about chemical components of the eight-ingredient Qishi powder, inputting the names, molecular formulas, relative molecular weights and fragment information of the chemical components into Shortcut to PeakView software to build a screening database; secondly, importing data acquired by mass spectrometry into Shortcut to PeakView software for automatic screening and matching; and finally, carrying out structural inference on the accurate mass number of the compound and mass spectrum fragmentation fragments and characteristic fragment ions by combining related documents, and determining a final screening result.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
the invention carries out preliminary chemical component activity analysis on the eight-ingredient Qishi powder for the first time by a UPLC-Q-TOF-MS method, establishes a method for efficiently separating various effective components under positive and negative ion modes by optimizing the extraction conditions, chromatographic conditions and mass spectrum conditions of the effective components, qualitatively analyzes the traditional Chinese medicine chemical active components of a sample by matching with the activity of a database, totally identifies 89 traditional Chinese medicine active components, and attributing the medicine sources of the 89 active components. The invention uses UPLC-Q-TOF-MS technology to systematically and accurately characterize chemical components in the eight-ingredient Qishi powder, provides data support for further developing pharmacokinetics and pharmacodynamics substance basic research of the prescription, and lays a theoretical foundation for clinical application.
Drawings
FIG. 1 is a total ion flow diagram (positive ion mode) of the eight-ingredient Qishisan UPLC-Q-TOF-MS in example 1.
FIG. 2 is a total ion flow chart (negative ion mode) of the eight-ingredient Qishisan UPLC-Q-TOF-MS in example 1.
FIG. 3 is a UPLC-Q-TOF-MS total ion flow diagram (positive ion mode) obtained by water extraction.
Fig. 4 is a general ion flow diagram (negative ion mode) of a UPLC-Q-TOF-MS obtained by adopting a water extraction mode.
Detailed Description
The present invention will be further described with reference to the following examples in order to more clearly illustrate the present invention.
1. Instrument and materials
1.1 Instrument BSA224S type 10-thousand electronic balance (Sartorius Corp., germany); triple TOF5600 high resolution time of flight mass spectrometer (AB SCIEX Co., USA).
1.2 materials eight ingredient zichongkusan, offered by affiliated hospitals at the university of Tibetan medicine; methanol, mass spectrum grade, formic acid, mass spectrum grade, acetonitrile, mass spectrum grade, purchased from Merck kgaa, germany; ultrapure water.
2. Examples
The experiment establishes a method for detecting main chemical components in the eight-ingredient Chinese mosla herb powder by adopting UPLC-Q-TOF-MS technology.
Example 1
The method for analyzing the multiple components in the eight-ingredient zichongkusan comprises the following steps:
s1, preparing a sample solution: adding 0.2g of Tibetan medicine Qixiao powder into a 10ml centrifuge tube, adding 5ml of 50% methanol solution into the centrifuge tube, shaking and mixing uniformly, performing ultrasonic treatment for 45min, centrifuging at 13000rpm for 10min, taking out supernatant, and passing through a 0.22 μm microporous filter membrane to obtain a sample solution;
s2, detecting and analyzing the sample solution by adopting a triple quadrupole time-of-flight high-resolution mass spectrum, wherein the detection conditions comprise:
chromatographic conditions: the chromatographic instrument is Shimadzu LC-30A, the chromatographic column is C18, the specification is 2.1mm multiplied by 100mm, and the size is 1.7 mu m; the column temperature is 45 ℃; the flow rate is 0.4ml/min; the sample injection amount is 4 μl; the mobile phase adopts a gradient elution program of acetonitrile-0.1% formic acid aqueous solution, and specifically comprises the following steps: 0-0.01 min,5% B; 0.01-15 min, 5-30% B; 15-35 min, 30-95% B; 35-37 min,95% B; 37-37.1 min, 95-5% B; 37.1-40 min, 5-0B; the concentrations are all volume percentages;
mass spectrometry conditions: mass spectrometry instrumentation was AB Sciex Triple TOF 5600+. The primary mass spectrum scanning is carried out, wherein the ionization mode is an electrospray positive ion mode, the ion source voltage is 5500V, the ion source temperature is 500 ℃, the declustering voltage is 100V, the collision energy is 35eV, and the collision energy is expanded to 15eV; the atomization gas is nitrogen, the auxiliary gas 1 is 50PSI, the auxiliary gas 2 is 50PSI, and the gas curtain gas is 40PSI; the scanning range of the primary mass spectrum parent ion is 50-1000, and the IDA sets 6 highest peaks with response values exceeding 100cps for secondary mass spectrum scanning; the scanning range of the sub-ions is 50-1000, dynamic background subtraction DBS is started, the ionization mode is an electrospray negative ion mode, the ion source voltage is-4500V, the ion source temperature is 500 ℃, the cluster removal voltage is 100V, the collision energy is-35 eV, and the collision energy is expanded to 15eV; the atomization gas is nitrogen, the auxiliary gas 1 is 50PSI, the auxiliary gas 2 is 50PSI, and the gas curtain gas is 40PSI; total ion maps were obtained, see fig. 1 and 2.
S3, referring to the literature to obtain data about chemical components of the Tibetan medicine eight-ingredient Qishi powder, and inputting the names, molecular formulas, relative molecular weights and fragment information about the chemical components into Shortcut to PeakView software to establish a screening database; data acquired by mass spectrometry is imported into Shortcut to PeakView software for automatic screening and matching; and carrying out structural inference on the accurate mass number of the compound and mass spectrum fragmentation fragments and characteristic fragment ions by combining related documents to determine a final screening result.
The invention refers to a large number of chemical component related literature reports of Tibetan medicine eight-ingredient Chinese mosla herb powder in the process of screening a database, and establishes a related prescription database by a traditional Chinese medicine system pharmacology database and analysis platform (TCMSP), a Chinese traditional medicine database retrieval system, and collecting Huang Huaxiang compound information of Chinese mosla herb, kola nut, common rabdosia herb, allium japonicum, tibetan rue, ash vegetable, radix angelicae pubescentis and artificial musk through combining Scifinder, pubchem and the like, so as to establish a related prescription database for 172 ingredients. The database contains compound names, molecular formulas, relative molecular weights, fragmentation information, etc. When Shortcut to PeakView software is adopted for automatic screening and matching, peaks with a response value of more than 1000 and within ppm+/-5 are selected in a positive ion mode, and 89 compounds are totally identified by utilizing the characteristic fragment ions of the obtained compounds and combining related documents for carrying out systematic analysis on the data. Details of analytical identification results are shown in Table 1 below.
The invention examines a plurality of extraction modes, including the traditional Chinese medicine water extraction and decoction mode and the methanol ultrasonic extraction mode. The steps of water extraction preparation for samples are as follows: 50g of eight-ingredient Chinese mosla herb powder and 10 times of water are taken for decoction for 2 hours, and the mixture is filtered by gauze, and filtrate is reserved. Decocting the residue with 10 times of water for 2 hr, collecting filtrate, mixing the filtrates, and storing in refrigerator at 4deg.C. The result shows that the active ingredients obtained by the traditional water extraction method are less than those obtained by the alcohol extraction method, so that the methanol-alcohol extraction method is adopted. Fig. 3 and 4 are the general ion flow diagrams of the UPLC-Q-TOF-MS obtained by water extraction and decoction.
The invention uses UPLC-Q-TOF-MS technology to systematically and accurately characterize chemical components in the eight-ingredient Qishi powder, provides data support for further developing pharmacokinetics and pharmacodynamics substance basic research of the prescription, and lays a theoretical foundation for clinical application.
The foregoing description is directed to the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the invention, and all equivalent changes or modifications made under the technical spirit of the present invention should be construed to fall within the scope of the present invention.
Claims (5)
1. The method for analyzing the multiple components in the eight-ingredient zichongkusan is characterized by comprising the following steps:
s1, preparing a sample solution: taking an eight-ingredient Chinese mosla herb powder sample, extracting active ingredients of the eight-ingredient Chinese mosla herb powder sample by using a methanol solution, wherein the ratio of feed liquid to extract is 0.2g:5ml, centrifuging the extracting solution to obtain supernatant, and passing through a membrane to obtain a sample solution;
s2, detecting and analyzing the sample solution by adopting a triple quadrupole time-of-flight high-resolution mass spectrum, wherein the detection conditions comprise:
chromatographic conditions: the chromatographic column is C18, the specification is 2.1mm multiplied by 100mm, and the specification is 1.7 mu m; the column temperature is 45 ℃; the flow rate is 0.4ml/min; the sample injection amount is 4 μl; the mobile phase adopts a gradient elution program of acetonitrile-0.1% formic acid aqueous solution, and specifically comprises the following steps: 0-0.01 min,5% B; 0.01-15 min, 5-30% B; 15-35 min, 30-95% B; 35-37 min,95% B; 37-37.1 min, 95-5% B; 37.1-40 min, 5-0B; the concentrations are all volume percentages;
mass spectrometry conditions: the primary mass spectrum scanning, wherein the ionization mode is an electrospray positive ion mode, the ion source voltage is 5500V, the ion source temperature is 500 ℃, the cluster removal voltage is 100V, the collision energy is 35eV, the collision energy is 15eV, the atomization gas is nitrogen, the auxiliary gas 1 is 50PSI, the auxiliary gas 2 is 50PSI, the gas curtain gas is 40PSI, the primary mass spectrum parent ion scanning range is 50-1000, and the IDA setting response value exceeds 6 highest peaks of 100cps to carry out secondary mass spectrum scanning; the scanning range of the sub-ions is 50-1000, dynamic background subtraction DBS is started, the ionization mode is an electrospray negative ion mode, the ion source voltage is-4500V, the ion source temperature is 500 ℃, the cluster removal voltage is 100V, the collision energy is-35 eV, and the collision energy is expanded to 15eV; the atomization gas is nitrogen, the auxiliary gas 1 is 50PSI, the auxiliary gas 2 is 50PSI, and the gas curtain gas is 40PSI;
s3, analyzing the data acquired by the mass spectrum, so as to analyze and identify the components of the eight-ingredient Chinese mosla herb powder.
2. The method for analyzing the multiple components in the eight-ingredient zichosla powder according to claim 1, which is characterized in that: in step S1, extraction is performed by using a methanol solution with a volume concentration of 50%.
3. The method for analyzing the multiple components in the eight-ingredient zichosla powder according to claim 1, which is characterized in that: in the step S1, the ultrasonic extraction mode is adopted for extraction, and the extraction time is 45 minutes.
4. The method for analyzing the multiple components in the eight-ingredient zichosla powder according to claim 1, which is characterized in that: the centrifugation in step S1 was performed at 13000rpm for 10min.
5. The method for analyzing the multiple components in the eight-ingredient zichosla powder according to claim 1, which is characterized in that: the analysis and identification method in the step S3 is as follows: first, referring to the literature to obtain data about chemical components of the eight-ingredient Qishi powder, inputting the names, molecular formulas, relative molecular weights and fragment information of the chemical components into Shortcut to PeakView software to build a screening database; secondly, importing data acquired by mass spectrometry into Shortcut to PeakView software for automatic screening and matching; and finally, carrying out structural inference on the accurate mass number of the compound and mass spectrum fragmentation fragments and characteristic fragment ions by combining related documents, and determining a final screening result.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108088926A (en) * | 2017-12-16 | 2018-05-29 | 中国农业科学院蔬菜花卉研究所 | A kind of method for detecting flavonoid components in tree peony blade |
| CN110455964A (en) * | 2019-10-14 | 2019-11-15 | 江西中医药大学 | The analysis of Coumarins ingredient and identification method in decomposite leaf Radix Angelicae Pubescentis alcohol extract |
| WO2020224471A1 (en) * | 2019-05-05 | 2020-11-12 | 江南大学 | Pretreatment method for ultrasonic-assisted extraction of various steroid hormones in sediments |
| CN112903841A (en) * | 2021-01-18 | 2021-06-04 | 中国检验检疫科学研究院 | Method for detecting isomers of chlorogenic acids |
| WO2022021886A1 (en) * | 2020-07-29 | 2022-02-03 | 石家庄以岭药业股份有限公司 | Method for separation and structural identification of relevant metabolites of lianhua qingwen drugs |
| CN114088829A (en) * | 2021-11-04 | 2022-02-25 | 天津中医药大学 | Detection method and application of dehydrocorydaline and metabolite thereof |
| WO2022110569A1 (en) * | 2020-11-27 | 2022-06-02 | 海南医学院 | Lc-ms/ms measurement method for aloesin in rat blood plasma |
| CN116242941A (en) * | 2023-03-13 | 2023-06-09 | 广州海关技术中心 | Analysis method for measuring 1,3, 7-trimethyl xanthine in cosmetics based on electrospray technology |
| WO2023193323A1 (en) * | 2022-04-08 | 2023-10-12 | 浙江大学医学院附属第一医院 | Rapid, comprehensive and stable identification method for unknown toxicants |
| CN117250300A (en) * | 2023-11-17 | 2023-12-19 | 江西中医药大学 | Method for detecting multiple components in Tibetan medicine twenty-five-flavor big soup pill |
| WO2024007531A1 (en) * | 2022-07-04 | 2024-01-11 | 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 simultaneously measuring content of 24 ingredients in daochi wan |
-
2024
- 2024-02-02 CN CN202410151064.5A patent/CN117686622B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108088926A (en) * | 2017-12-16 | 2018-05-29 | 中国农业科学院蔬菜花卉研究所 | A kind of method for detecting flavonoid components in tree peony blade |
| WO2020224471A1 (en) * | 2019-05-05 | 2020-11-12 | 江南大学 | Pretreatment method for ultrasonic-assisted extraction of various steroid hormones in sediments |
| CN110455964A (en) * | 2019-10-14 | 2019-11-15 | 江西中医药大学 | The analysis of Coumarins ingredient and identification method in decomposite leaf Radix Angelicae Pubescentis alcohol extract |
| WO2022021886A1 (en) * | 2020-07-29 | 2022-02-03 | 石家庄以岭药业股份有限公司 | Method for separation and structural identification of relevant metabolites of lianhua qingwen drugs |
| WO2022110569A1 (en) * | 2020-11-27 | 2022-06-02 | 海南医学院 | Lc-ms/ms measurement method for aloesin in rat blood plasma |
| CN112903841A (en) * | 2021-01-18 | 2021-06-04 | 中国检验检疫科学研究院 | Method for detecting isomers of chlorogenic acids |
| CN114088829A (en) * | 2021-11-04 | 2022-02-25 | 天津中医药大学 | Detection method and application of dehydrocorydaline and metabolite thereof |
| WO2023193323A1 (en) * | 2022-04-08 | 2023-10-12 | 浙江大学医学院附属第一医院 | Rapid, comprehensive and stable identification method for unknown toxicants |
| WO2024007531A1 (en) * | 2022-07-04 | 2024-01-11 | 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 simultaneously measuring content of 24 ingredients in daochi wan |
| CN116242941A (en) * | 2023-03-13 | 2023-06-09 | 广州海关技术中心 | Analysis method for measuring 1,3, 7-trimethyl xanthine in cosmetics based on electrospray technology |
| CN117250300A (en) * | 2023-11-17 | 2023-12-19 | 江西中医药大学 | Method for detecting multiple components in Tibetan medicine twenty-five-flavor big soup pill |
Non-Patent Citations (6)
| Title |
|---|
| 何潇;伍慧敏;熊乐乐;金红利;刘艳芳;沈爱金;梁鑫淼: "基于UPLC-Q-TOF-MS技术的赤芍单萜类成分研究", 中国中药杂志, vol. 48, no. 004, 31 December 2023 (2023-12-31) * |
| 刘天浩;羊忠山;李宁;吴月滢;韩思思;韩妮萍;袁嘉丽;: "基于UPLC-MS/MS对肺系调治方化学成分的研究", 时珍国医国药, no. 01, 30 April 2020 (2020-04-30) * |
| 夏丽文;彭丽萍;杨东华;徐立亭;: "超高效液相色谱-电喷雾飞行时间质谱分析五味子化学成分", 中医药信息, no. 04, 10 July 2012 (2012-07-10) * |
| 李洋;余静;赵亚红;安泳潼;薛丹;柴逸峰;张国庆;张海;: "中药复方制剂八宝丹中化学成分的UHPLC-Q-TOF/MS分析", 第二军医大学学报, no. 12, 20 December 2016 (2016-12-20) * |
| 白海玉;刘宝忠;霍金海;: "基于液质联用技术的野菊花中黄酮成分分析", 中国中医药科技, no. 06, 20 November 2018 (2018-11-20) * |
| 范姣姣;文红梅;单晨啸;周红光;陈海彬;吴勉华;: "基于UFLC-Q-TOF/MS技术的八月札化学成分研究", 中草药, no. 23, 12 December 2013 (2013-12-12) * |
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