CN107607654B - Method for analyzing flavonoid chemical components in walnut flower - Google Patents
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Abstract
The invention discloses a method for analyzing the chemical components of flavonoids in walnut flowers, which comprises the following steps: extracting a walnut flower medicinal material by adopting an ethanol heating reflux method, concentrating, redissolving, carrying out ultrasonic treatment, filtering to obtain a test solution, detecting the test solution by adopting an ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry method to obtain second-level mass spectrum information of a compound, and analyzing chemical component information in a detection result. The method can quickly and efficiently analyze the flavonoid compounds in the walnut flower, provides a basis for the research and the quick and accurate identification of the drug effect substances of the walnut flower, and is beneficial to the development and the utilization of the walnut flower.
Description
Technical Field
The invention relates to a method for analyzing chemical components, in particular to a method for analyzing flavonoid chemical components in walnut flowers based on an ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry technology.
Background
The walnut flower is the flower column of walnut, also called walnut nutlet, longevity vegetable, asparagus. The medicinal liquor is eaten as a cold dish by folks and is clinically prepared into a tincture for removing warts. Its main components include linoleic acid glyceride, protein, carbohydrate and vitamins, etc., and has the functions of promoting hemopoiesis of human body, preventing arteriosclerosis, relieving asthma and moistening intestines. At present, the research on the components of the walnut flower mainly comprises flavonoid compounds, and no report about the analysis of the flavonoid chemical components in the walnut flower by adopting an ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry technology exists.
Disclosure of Invention
The invention aims to provide a method for analyzing the chemical components of the flavonoids in the walnut flowers, which provides a rapid and efficient analysis method for analyzing the chemical components of the flavonoids in the walnut flowers by an ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (ULLC-MS/MS) technology.
A method for detecting flavonoid chemical components in walnut flowers comprises the following steps:
extracting a walnut flower medicinal material by adopting an ethanol heating reflux method, concentrating, redissolving, carrying out ultrasonic treatment, filtering to obtain a test solution, and detecting the test solution by adopting an ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry method.
The invention relates to a method for detecting flavonoid chemical components in walnut flowers, wherein the analysis TF1.7.1 software is used for setting chromatographic conditions in the ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry method, and the parameters are as follows:
the chromatographic column is ACQUITY BEH C18100mm × 2.1.1 mm, 1.7 mu m, 0.1 percent formic acid-water as a mobile phase A, methanol as a mobile phase B, linear gradient elution for 0-1 min, 20-35 percent B, 1 min-5 min, 35-80 percent B, 5 min-15 min, 80-100 percent B, 15 min-17 min, 100 percent B, 17.1 min-20 min,20 percent B, volume flow of 0.4m L/min, column temperature of 40 ℃ and sample injection amount of 10 mu L.
The invention relates to a method for detecting flavonoid chemical components in walnut flowers, wherein Analyst TF1.7.1 software is used for setting mass spectrum conditions in the ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrum method, and the parameters are set as follows:
UP L C-Triple-TOF 5600+ flight time LC-MS instrument with positive ion scanning mode, m/z 100-1200, ion source temperature 150 deg.C, ion source voltage 4500V and desolvation gas N2: 110 psi; temperature of the desolventizing gas: 600 ℃; air curtain gas N2: 35 psi; primary scanning: declustering voltage DP: 80V; secondary scanning: and collecting mass spectrum data by using TOF MS-Product Ion-IDA modes, wherein the CID energy is 20-50 eV.
The method for detecting the flavonoid chemical components in the walnut flower specifically comprises the following steps of taking a flask containing 1.0g to 50m L of walnut flower medicinal materials, heating and refluxing 50m L50% ethanol for 2 times, extracting for the first time for 30min, extracting for the second time for 1h, filtering, combining two filtrates, concentrating under reduced pressure to be dry, redissolving 5m L methanol, carrying out ultrasonic treatment for 30min, supplementing the total weight of the filtrate with methanol, filtering with a 0.22-micron microporous filter membrane, and storing the filtrate in a refrigerator at 4 ℃ as a test solution.
A method for analyzing flavonoid chemical components in walnut flowers comprises the following steps: the method is adopted to detect the flavonoid chemical components in the walnut flower, so as to obtain the total ion flow diagram, the first-level mass spectrum information and the second-level mass spectrum information of the compound, and the chemical component information in the detection result is analyzed by applying PeakView2.2 software, wherein the PeakView2.2 comprises a MasterView 1.1 plug-in:
(1) the information of the collected walnut flower samples is recorded in MasterView 1.1, and the analysis parameters are set as follows: intensity (response value): >1000 counts; s: N (Signal-to-noise ratio): > 10; default XIC Width (extracted ion Width): 0.02 Da; default Retention Time Width (Retention Time Width): 2 min; default Threshold: 100 cps; minimum Retention Time (Minimum Retention Time): 0.3 min; mass Error (molecular weight Error): <10 ppm;
(2) introducing the molecular formula into MasterView 1.1 according to the existing database containing flavonoid compounds in 948 Chinese medicinal materials and the flavone compounds found in Juglans reported in the literature, and setting each flavonoid compound in the MasterView 1.1The addition form of the molecular ions of the compound is [ M + H]+Or [ M + Na]+Matching with walnut flower data by using MasterView 1.1 according to the molecular formula and the molecular weight to obtain a result list of matching of all introduced compound information and data obtained by experiments; the compound information which meets the parameters set in the step (1) in the result shows green, and the compound which meets the parameters set in the step (1) does not show green if the compound information does not meet the parameters set in the step (1), the compound which meets the parameters set in the result is screened out through MasterView 1.1 software, and the information in the compound list which meets the parameters set is derived, wherein the information comprises Formula (molecular Formula), Mass (theoretical molecular weight), Adduct (actual molecular weight), Extraction (addition form), Error (Error), Intensity (response value) and Found At RT (retention time);
simultaneously, the information of each clicked compound is exported one by one and the first-order mass spectrogram and the second-order mass spectrogram which are displayed in MasterView 1.1 and correspond to the clicked compound are saved so as to facilitate the next analysis;
(3) in order to prevent database and literature reported compounds from being filtered for valid information due to errors during software matching, the Mass Error in the parameters set in step (1): <10ppm, this range is large, therefore further analysis and screening one by one is required;
calculating the accurate mass number of molecular ions of each compound molecular formula by using analysis TF1.7.1, Calculators and Isotropic Distribution, and calculating the first-order mass spectrum information of the compound recorded in the step (2) according to the formula:
error (ppm) ═ actual molecular weight-theoretical molecular weight)/theoretical molecular weight × 106
Removing compounds with error of more than 5 ppm;
(4) in order to improve the reliability of identification, performing secondary mass spectrometry on the result obtained after removing part of the compounds in the step (3): and (3) analyzing the cracking way of the compound according to a literature, an mzCloud mass spectrum database and the cracking rule of the flavonoid compound, and if two fragment ions in the secondary mass spectrum information obtained in the experiment accord with the cracking rule of the compound and the error range of the actual molecular weight and the theoretical molecular weight of the fragment ions is less than 15ppm, determining that the compound exists in the experimental sample, wherein the error calculation formula is the same as that in the step (3).
The method for analyzing the flavonoid chemical components in the walnut flowers is different from the prior art in that:
the method for analyzing the flavonoid chemical components in the walnut flowers uses UHP L C-Triple-TOF-MS for the first time to analyze and measure the flavonoid chemical components, provides a quick and efficient identification method for identifying the chemical components in the walnut flowers, and provides technical reference for basic research and quality control of pharmacodynamic substances of the chemical components in the walnut flowers.
The method for analyzing the flavonoid chemical components in the walnut flower is further explained by combining the attached drawing.
Drawings
FIG. 1 is a ion flow diagram for extracting 36 compounds in the example of the present invention.
Detailed Description
Instrument and material
The walnut flower sample is identified as walnut flower column of juglans plant of juglans genus of Juglans of Juglandaceae family by professor Rehai Min of Beijing university of traditional Chinese medicine; methanol and formic acid were chromatographically pure (PA company, USA), water was Milli-Q ultrapure water, and the rest of the reagents were analytically pure (Beijing chemical plant company).
UP L C-Triple-TOF/MS System Exion L CTMModel AD high performance liquid chromatograph (AB SCIEX, USA), Triple TOF 5600+Mass spectrometer equipped with ESI ion source (AB SCIEX, USA)
Secondly, a method for detecting the chemical components of the flavonoids in the walnut flowers comprises the following steps:
1. chromatographic and mass spectral conditions
The chromatographic condition of the chromatographic column is ACQUITY BEH C18(100mm × 2.1.1 mm, 1.7 mu m), 0.1 percent formic acid-water as a mobile phase A, methanol as a mobile phase B, linear gradient elution for 0-1 min, 20-35 percent B, 1 min-5 min, 35-80 percent B, 5 min-15 min, 80-100 percent B, 15 min-17 min, 100 percent B, 17.1 min-20 min,20 percent B, volume flow of 0.4m L/min, column temperature of 40 ℃ and sample injection amount of 10 mu L.
Mass spectrum condition UP L C-Triple-TOF 5600+Time-of-flight LC-MS: a positive ion scanning mode; scanning range: m/z is 100-1200; (ii) a Ion source temperature: 150 ℃; ion source voltage: 4500V; desolventizing gas (N)2): 110 psi; temperature of the desolventizing gas: 600 ℃; air curtain gas (N)2): 35 psi; primary scanning: declustering voltage (DP): 80V; secondary scanning: collecting mass spectrum data by using TOF MS-Product Ion-IDA modes, wherein CID energy is 20-50 eV; data analysis software: analyst TF1.7.1, PeakView2.2, and MasterView 1.1.
2. Preparation of test solution
Taking a flask containing walnut anther 1.0g to 50m L, heating and refluxing with 50m L50% ethanol for 2 times, extracting for the first time for 30min, extracting for the second time for 1h, filtering, combining the two filtrates, concentrating under reduced pressure to dryness, redissolving with 5m L methanol, performing ultrasound for 30min, supplementing with methanol to the original total weight, filtering with 0.22 μm microporous membrane, and storing in a refrigerator at 4 deg.C as a test solution.
Analysis method of flavonoid chemical components in walnut flower
The method is adopted to detect the flavonoid chemical components in the walnut flower, so as to obtain the total ion flow diagram, the first-level mass spectrum information and the second-level mass spectrum information of the compound, and the chemical component information in the detection result is analyzed by applying PeakView2.2 software, wherein the PeakView2.2 comprises a MasterView 1.1 plug-in:
(1) the information of the collected walnut flower samples is recorded in MasterView 1.1, and the analysis parameters are set as follows: intensity: >1000 counts; s, N: > 10; default XIC Width: 0.02 Da; default Retention TimeWidth: 2 min; default Threshold: 100 cps; minimum Retention Time: 0.3 min; mass Error: <10 ppm;
(2) according to the existing database containing flavonoid compounds in 948 traditional Chinese medicines and the existing literature reports that the flavonoid compounds found in Juglans are taken as the basis, the molecular formula of the flavonoid compounds is introduced into MasterView 1.1, and the addition form (addition) of each compound molecular ion is set to be [ M + H ] in the MasterView 1.1]+Or [ M + Na]+Matching with walnut flower data by using MasterView 1.1 according to molecular formula and molecular weight to obtainA result list of all the imported compound information matched with the data obtained by the experiment; the compound information which meets the set parameters in the step (1) in the result shows green, if the compound information does not meet the set parameters, the compound which meets the set parameters in the result, namely the compound which is shown as green, is screened out through MasterView 1.1 software, and the information in the compound list which meets the set parameters is exported, wherein the information comprises Formula, Mass, Adduct, Extraction, Error, Intensity and Found AtRT;
simultaneously, the information of each clicked compound is exported one by one and the first-order mass spectrogram and the second-order mass spectrogram which are displayed in MasterView 1.1 and correspond to the clicked compound are saved so as to facilitate the next analysis;
(3) in order to prevent the database and the literature-reported compound from filtering the valid information due to errors in the software matching process, the Mass Error: <10ppm, this range is large, therefore further analysis and screening one by one is required;
calculating the accurate mass number of molecular ions of each compound molecular formula by using analysis TF1.7.1, Calculators, Isotropic Distribution, and the information of the primary mass spectrum of the compound recorded in (2), according to the formula:
error (ppm) ═ actual molecular weight-theoretical molecular weight)/theoretical molecular weight × 106
Removing compounds with error of more than 5 ppm;
(4) in order to improve the reliability of identification, performing secondary mass spectrometry on the result obtained after removing part of the compounds in the step (3): according to the literature, an mzCloud mass spectrum database and the cracking rule analysis of flavonoids compounds, if the two-stage mass spectrum information obtained in the experiment has two fragment ions (the flavonoid glycoside compound has at least one fragment ion because the volatile glycosyl group obtains one aglycone fragment ion) which accord with the cracking rule of the compounds, and the error range of the actual molecular weight and the theoretical molecular weight of the fragment ions is less than 15ppm (the error calculation formula is the same as (3)), the compound is considered to exist in the experimental sample.
According to the analysis method, 36 flavonoid compounds in the walnut flower are identified in total, and 25 compounds are presumed not reported in the prior literature. The additive diagram of the ion flow diagram is extracted, as shown in figure 1, and the relevant information of 36 compounds is shown in table 1.
Fourth, optimization of experimental method
1. Extraction method, time and solvent selection
Comparing two extraction methods of ultrasonic extraction and heating reflux extraction, extracting within 20-60 min, and respectively extracting with 50% methanol, 50% ethanol, 80% methanol and 80% ethanol, and comparing the extraction efficiency of the walnut flower extract under different conditions. The result shows that the extraction efficiency is higher when 50 percent ethanol is heated and refluxed for 30 min.
2. Chromatographic column selection
Comparison of ACQUITY BEH C under the same experimental conditions18(100mm×2.1mm，1.7μm),ACQUITY BEHC18(150mm × 2.1.2.1 mm, 1.7 μm) and ACQUITY HSS C18(100mm × 2.1mm, 1.8 μm) separation efficiency of three columns BEH type column can provide better separation efficiency and peak shape for most compounds, and has universality ACQUITYHSS C18(100mm × 2.1mm, 1.8 μm) relative to ACQUITY BEH C18(100mm × 2.1mm, 1.7 μm) separation efficiency was low, while ACQUITY BEH C18(150mm × 2.1mm, 1.7 μm) results in a higher column pressure.
Fifth, conclusion
In the experiment, UHP L C-Triple-TOF-MS is adopted to rapidly analyze flavonoids compounds in walnut flower products in a positive ion mode, 36 flavonoids compounds are conjectured, 25 of the flavonoids compounds are not reported in the past documents, and certain reference is provided for further chemical composition, pharmacological research and quantitative research.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (4)
1. A method for detecting flavonoid chemical components in walnut flowers is characterized by comprising the following steps: the method comprises the following steps:
extracting a walnut flower medicinal material by adopting a 50% ethanol heating reflux method, concentrating, redissolving, carrying out ultrasonic treatment, filtering to obtain a test sample solution, and detecting the test sample solution by adopting an ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry method;
and (3) setting chromatographic conditions in the ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry method by applying analysis TF1.7.1 software, wherein the parameters are set as follows:
the chromatographic column is ACQUITY BEH C18100mm × 2.1.1 mm, 1.7 mu m, 0.1 percent formic acid-water as a mobile phase A, methanol as a mobile phase B, linear gradient elution for 0-1 min, 20-35 percent B, 1 min-5 min, 35-80 percent B, 5 min-15 min, 80-100 percent B, 15 min-17 min, 100 percent B, 17.1 min-20 min,20 percent B, volume flow of 0.4m L/min, column temperature of 40 ℃ and sample injection amount of 10 mu L.
2. The method for detecting the flavonoid chemical components in the walnut flowers according to claim 1, characterized in that: and (3) setting mass spectrum conditions in the ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry method by applying analysis TF1.7.1 software, wherein the parameters are set as follows:
UP L C-Triple-TOF 5600+ time-of-flight LC-MS (liquid chromatography-Mass spectrometer) instrument with positive ion scanning mode and scanning range: m/z is 100-1200; ion source temperature: 150 ℃; ion source voltage: 4500V; desolventizing gas N2: 110 psi; temperature of the desolventizing gas: 600 ℃; air curtain gas N2: 35 psi; primary scanning: declustering voltage DP: 80V; secondary scanning: and collecting mass spectrum data by using TOF MS-Product Ion-IDA modes, wherein the CID energy is 20-50 eV.
3. The method for detecting the flavonoid chemical components in the walnut flowers as claimed in claim 2, wherein the preparation of the test solution specifically comprises the steps of taking 1.0g to 50m L flask of walnut flower medicinal materials, heating and refluxing with 50m L50% ethanol for 2 times, carrying out first extraction for 30min and second extraction for 1h, filtering, combining two filtrates, concentrating under reduced pressure to dryness, carrying out 5m L methanol redissolution, carrying out ultrasonic treatment for 30min, supplementing the total weight with methanol, carrying out 0.22 μm microporous membrane filtration, and storing in a refrigerator at 4 ℃ as a test solution.
4. A method for analyzing the flavonoid chemical components in walnut flowers is characterized by comprising the following steps: the method comprises the following steps: the method of claim 2 is adopted to detect flavonoid chemical components in walnut flowers, a total ion flow diagram, first-level mass spectrum information and second-level mass spectrum information of the compounds are obtained, PeakView2.2 software is applied to analyze the chemical component information in the detection result, and the PeakView2.2 comprises a MasterView 1.1 plug-in:
(1) the information of the collected walnut flower samples is recorded in MasterView 1.1, and the analysis parameters are set as follows: response value >1000 counts; signal-to-noise ratio: > 10; and (3) extracting ion width: 0.02 Da; retention time width: 2 min; threshold value: 100 cps; minimum retention time: 0.3 min; error in molecular weight: <10 ppm;
(2) according to the existing database containing flavonoid compounds in 948 traditional Chinese medicines and the existing literature reports that the flavonoid compounds found in Juglans are taken as the basis, the molecular formula of the flavonoid compounds is introduced into MasterView 1.1, and the addition form of molecular ions of each compound is set as [ M + H ] in the MasterView 1.1]+Or [ M + Na]+Matching with walnut flower data by using MasterView 1.1 according to molecular formula and molecular weightObtaining a result list of matching all the imported compound information with the data obtained by the experiment; the compound information which accords with the parameters set in the step (1) in the result shows green, and does not show green if the compound information does not accord with the parameters set in the step (1), the compound which accords with the parameter set in the result, namely the compound which shows green, is screened out through MasterView 1.1 software, and the information in the compound list which accords with the parameter set is exported, wherein the information comprises a molecular formula, a theoretical molecular weight, an actual molecular weight, an addition form, an error, a response value and retention time;
simultaneously, the information of each clicked compound is exported one by one and the first-order mass spectrogram and the second-order mass spectrogram which are displayed in MasterView 1.1 and correspond to the clicked compound are saved so as to facilitate the next analysis;
(3) in order to prevent database and literature reported compounds from being filtered for valid information due to errors during software matching, the molecular weight error in the parameters set in step (1): <10ppm, this range is large, therefore further analysis and screening one by one is required;
calculating the accurate mass number of molecular ions of each compound molecular formula by using analysis TF1.7.1 > computers > Isotropic Distribution software, and the information of the first-order mass spectrum of the compound recorded in the step (2), according to the formula:
error ppm (actual molecular weight-theoretical molecular weight)/theoretical molecular weight × 106
Removing compounds with error of more than 5 ppm;
(4) in order to improve the reliability of identification, performing secondary mass spectrometry on the result obtained after removing part of the compounds in the step (3): and (3) analyzing the cracking way of the compound according to a literature, an mzCloud mass spectrum database and the cracking rule of the flavonoid compound, and if two fragment ions in the secondary mass spectrum information obtained in the experiment accord with the cracking rule of the compound and the error range of the actual molecular weight and the theoretical molecular weight of the fragment ions is less than 15ppm, determining that the compound exists in the experimental sample, wherein the error calculation formula is the same as that in the step (3).
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| 基于 UPLC-Q-TOF/MS 技术的核桃楸皮成分分析;孙国东等;《中草药》;20170228;第48卷(第4期);第657-667页 * |
| 基于超高效液相-四级杆-飞行时间串联质谱的白花蛇舌草注射液主成分分析;张亚中;《中草药》;20130430;第44卷(第7期);全文 * |
| 核桃花中总黄酮的含量测定研究;李少泓;《中华中医药学刊》;20120430;第30卷(第4期);第915-917页 * |
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