CN113533553A - Roxburgh rose and product component detection method thereof and method for establishing Roxburgh rose component database - Google Patents

Roxburgh rose and product component detection method thereof and method for establishing Roxburgh rose component database Download PDF

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CN113533553A
CN113533553A CN202110639729.3A CN202110639729A CN113533553A CN 113533553 A CN113533553 A CN 113533553A CN 202110639729 A CN202110639729 A CN 202110639729A CN 113533553 A CN113533553 A CN 113533553A
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roxburgh rose
rosa roxburghii
mobile phase
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solution
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CN113533553B (en
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孙宝清
徐文流
伍建林
颜冠裕
翁少全
张毅达
郑佩燕
李词周
郑荣波
王宇
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Guangzhou Wanglaoji Major Health Industry Co ltd
First Affiliated Hospital of Guangzhou Medical University
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Guangzhou Wanglaoji Major Health Industry Co ltd
First Affiliated Hospital of Guangzhou Medical University
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
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Abstract

The invention discloses a method for detecting the components of roxburgh rose and products thereof and a method for establishing a roxburgh rose component database. The invention is based on LC-MS/MS technology, realizes real-time, rapid and economic detection of roxburgh rose sample components, and in addition, the existing data resources are utilized to compare and identify with LC-MS/MS results, the obtained identification results are established into a roxburgh rose database, and different roxburgh rose samples are used to verify the database, so that the quality analysis of each roxburgh rose sample is synchronously realized, the control of roxburgh rose product quality is facilitated, and the further excavation of roxburgh rose efficacy is facilitated.

Description

Roxburgh rose and product component detection method thereof and method for establishing Roxburgh rose component database
Technical Field
The invention relates to a method for detecting components of roxburgh rose and products thereof and a method for establishing a roxburgh rose component database.
Background
Rosa roxburghii (Rosa roxburghii) is a perennial deciduous shrub of the genus Rosa of the family Rosaceae, and is called "the king of vitamin C" in the fruit kingdom. According to the records of the compendium of materia medica, the fruit of rosa roxburghii tratt is also an ancient Chinese medicament, is used for treating folk diseases and has the property of homology of medicine and food. The roxburgh rose has unique fruit fragrance and high nutritional value, and in recent years, the pharmacological actions of the roxburgh rose are reported one by one and comprise antitumor activity, anti-inflammatory activity, anti-apoptosis activity, radiation protection, anti-atherosclerosis and oxidation resistance. At present, the research on the components of the roxburgh rose shows that the roxburgh rose is rich in vitamin C, flavonoid compounds, polysaccharide, organic acid, triterpene, trace elements, superoxide dismutase, amino acid and other components. However, at present, the analysis of the components of the rosa roxburghii tratt is basically carried out by combining LC-MS, GC-MS and HPLC with standard substances, a large number of standard substances are required to be purchased, various types of components cannot be detected simultaneously, if the components need to be detected, different equipment needs to be used under different experimental conditions, the detection error is high, more equipment cost, experimental cost and time cost need to be consumed, and the method is not suitable for realizing real-time and economic quality control in the production process.
Besides fresh roxburgh rose, a plurality of processing products of roxburgh rose, such as roxburgh rose preserved fruit, roxburgh rose powder, roxburgh rose dry and the like, are also on the market at present. At present, the production of the rosa roxburghii tratt basically depends on the familiarity of one family from planting, managing, picking, processing and selling, the rosa roxburghii tratt industry does not get rid of the low-end processing industry with intensive labor force and low added value developed by the use of the population dividend, and the monitoring of effective components and safety components in the production process of raw materials, intermediate products and finished products is lacked. In addition, "the deep processing of roxburgh rose is promoted" in "the white skin book developed by roxburgh rose industry in Guizhou province. A series of intensive processing projects of medicinal and edible dual-purpose industries such as rosa roxburghii tratt medicated diet, medicinal liquor, medicinal tea, health care products and the like are implemented, enterprises are supported to develop rosa roxburghii tratt additives, skin care products, hair washing products, toothpaste products and the like, and a long rosa roxburghii tratt industrial chain is made, so that the industrial breadth is widened.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for detecting the components of roxburgh rose and products thereof and a method for establishing a roxburgh rose component database, so as to realize real-time, quick and economic detection of roxburgh rose raw materials and the components of the products thereof and be conductive to the control of the quality of roxburgh rose products.
In order to achieve the above object, in a first aspect, the present invention provides a method for detecting the components of a sample of rosa roxburghii tratt, which comprises the following steps:
(1) processing a roxburgh rose sample to obtain a test sample solution;
(2) injecting the test solution into a liquid phase tandem mass spectrometer for detection;
wherein, the liquid phase conditions are as follows: the chromatographic column is a C18 chromatographic column, the mobile phase consists of a mobile phase A and a mobile phase B, the mobile phase A is formic acid aqueous solution with the volume concentration of 0.05-0.2%, the mobile phase B is formic acid acetonitrile solution with the volume concentration of 0.05-0.2%, gradient elution is carried out, the flow rate is 0.1-1 mL/min, and the column temperature is 30-50 ℃;
the mass spectrometry conditions were as follows: selecting an electrospray ion source, a positive and negative ion mode and positive ion source parameters: the temperature of the sheath gas is 240-260 ℃, the flow rate of the sheath gas is 10-12L/min, the temperature of the auxiliary gas is 140-160 ℃, the flow rate of the auxiliary gas is 14-16L/min, the air pressure of a sprayer is 23-27 psi, the voltage of a capillary tube is 3800-4200V, and the collision energy is 10-40 eV; negative ion source parameters: the temperature of the sheath gas is 310-330 ℃, the flow rate of the sheath gas is 10-12L/min, the temperature of the auxiliary gas is 140-160 ℃, the flow rate of the auxiliary gas is 14-16L/min, the air pressure of the sprayer is 43-47 psi, the voltage of the capillary tube is 3300-3700V, and the collision energy is 10-40 eV;
the roxburgh rose sample is roxburgh rose or a product thereof. Examples of the Rosa roxburghii product include Rosa roxburghii extract, Rosa roxburghii raw juice, Rosa roxburghii concentrated solution, and Rosa roxburghii juice, but the kind of Rosa roxburghii product is not limited thereto. Herein, "aqueous formic acid solution" refers to a solution prepared from formic acid and water, and "acetonitrile formic acid solution" refers to a solution prepared from formic acid and acetonitrile, and the similar descriptions apply to the same reason.
The detection method adopts LC-MS/MS technology which has high sensitivity and high analysis speed and is suitable for basic research of traditional Chinese medicine substances to identify the components in the roxburgh rose sample, thereby being beneficial to controlling the quality of the roxburgh rose and products thereof in the future, standardizing an industrial chain, guiding or optimizing the production and processing method of the roxburgh rose industry and further mining the efficacy of the roxburgh rose. In addition, the detection method can determine the components of the roxburgh rose sample without a standard substance, greatly saves the test cost, and can identify more than 120 components in the roxburgh rose.
Preferably, the gradient elution procedure is: the volume fraction of the mobile phase B is changed from 5% to 30% in 0-5 min; 5-10min, the volume fraction of the mobile phase B is changed from 30% to 70%; the volume fraction of the mobile phase B is changed from 70% to 95% in 10-11 min; 11-12min, the volume fraction of the mobile phase B is kept 95%; 12-12.1min, the volume fraction of the mobile phase B is changed from 95% to 5%; 12.1-14min, the volume fraction of mobile phase B is kept 5%. By adopting the liquid phase processing method, the detection time of the components of the roxburgh rose sample can be shortened to 14min, and the time cost is greatly saved.
Preferably, the step (2) is carried out according to the following liquid phase and mass spectrum conditions:
liquid phase: the mobile phase A is formic acid aqueous solution with volume concentration of 0.1 percent, and the mobile phase B is formic acid acetonitrile solution with volume concentration of 0.1 percent;
mass spectrometry positive ion source parameters: the temperature of the sheath gas is 250 ℃, the flow rate of the sheath gas is 11L/min, the temperature of the auxiliary gas is 150 ℃, the flow rate of the auxiliary gas is 15L/min, the air pressure of a sprayer is 25psi, the voltage of a capillary tube is 4000V, and the collision energy is 10-40 eV;
mass spectrum anion source parameters: the temperature of the sheath gas is 320 ℃, the flow rate of the sheath gas is 11L/min, the temperature of the auxiliary gas is 150 ℃, the flow rate of the auxiliary gas is 15L/min, the air pressure of the sprayer is 45psi, the voltage of the capillary tube is 3500V, and the collision energy is 10-40 eV.
Preferably, the column has a length of 100mm, a diameter of 2.1mm and a packing particle size of 1.7 μm.
Preferably, the roxburgh rose sample is roxburgh rose, roxburgh rose extract, roxburgh rose concentrate or roxburgh rose juice. The Rosa roxburghii juice can be obtained by squeezing or other methods.
Preferably, the sample of Rosa roxburghii Tratt is Rosa roxburghii Tratt; the step (1) is as follows: juicing the whole roxburgh rose, and carrying out solid-liquid separation to obtain a solution, namely a test solution.
Preferably, the sample of Rosa roxburghii Tratt is Rosa roxburghii Tratt; the step (1) is as follows: crushing Rosa roxburghii, extracting with water, collecting the extractive solution, concentrating, dissolving with acetonitrile water solution, and performing solid-liquid separation to obtain a sample solution.
Preferably, the roxburgh rose sample is roxburgh rose concentrated solution; the step (1) is as follows: and (3) carrying out solid-liquid separation on the roxburgh rose sample to obtain a solution, namely the test sample solution.
In a second aspect, the invention further provides a method for establishing a rosa roxburghii tratt component database, which comprises the following steps:
(S1) detecting the roxburgh rose sample according to the detection method;
(S2) analyzing the LC-MS/MS data obtained in the step (S1) in combination with existing databases and literature to identify the components of the rosa roxburghii tratt sample, and recording molecular formulas, relative retention times, parent ions and ion data of each identified component to obtain a rosa roxburghii tratt component database. The roxburgh rose component database established according to the method has more than 120 roxburgh rose components at present, and is more than the reports of the prior literature.
In step (S2), databases used are, for example, HMDB (https:// HMDB. ca /), Pubchem (https:// Pubchem. ncbi. nlm. nih. gov /), METLIN (https:// METLIN. scripts. edu/index. ph), Scifinder (sciferide. cas. org /), etc.
Preferably, the establishing method further comprises the steps of: different roxburgh rose samples are detected to verify the applicability of the LC-MS/MS method and the roxburgh rose component database.
Preferably, the establishing method further comprises the steps of: and presenting the verified roxburgh rose component database for the user to use. The presentation form may be selected as a WeChat applet, a Web page, H5, or the like.
Compared with the prior art, the invention has the beneficial effects that:
(1) in the prior art, standard products are required to be purchased for detecting the components of the roxburgh rose, but the detection method does not need the standard products, so that the test cost is greatly saved;
(2) the literature reports that the detection time of the roxburgh rose components is about 40min generally, and the optimization of the detection method can shorten the detection time to 14min, so that the detection is faster and more efficient;
(3) the rosa roxburghii ingredient database constructed by the invention has more than 120 ingredients at present, and is more than reported in the literature.
Drawings
FIG. 1 is a total ion flow diagram of the concentrated juice and the aqueous extract of Rosa roxburghii Tratt obtained in example 1;
FIG. 2 is a total ion flow diagram of Citrobacter spinosus;
FIG. 3 is a total ion flow diagram of raw roxburgh rose juice;
FIG. 4 shows the identification of a part of the ingredients common to Roxburgh Rose and Roxburgh Rose juice by the Roxburgh Rose ingredient database established in example 2.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1
The embodiment provides a method for detecting the components of a roxburgh rose sample, which comprises the following steps:
(1) preparing and pretreating a roxburgh rose water extract: weighing Rosa roxburghii Tratt, crushing, adding drinking water according to a material-liquid ratio of 1g:10mL, extracting for 1h by micro boiling, filtering, collecting filtrate, adding drinking water into filter residue according to a material-liquid ratio of 1g:8mL, extracting for 1h by micro boiling, filtering, combining the filtrates for 2 times, concentrating, dissolving 100 mu L of obtained concentrated solution with 1mL of 50% (v/v) acetonitrile-water solution, centrifuging at 13500rpm at normal temperature for 5min, and taking supernatant for subsequent detection;
(2) pretreatment of the roxburgh rose concentrated solution: centrifuging 1mL of the roxburgh rose concentrated solution at 13500rpm for 5 minutes at normal temperature, and taking the supernatant for subsequent detection;
(3) respectively injecting the supernatant obtained in the step (1) and the supernatant obtained in the step (2) into an Agilent ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometer (UHPLC-Q-TOF-MS) for detection,
wherein, the liquid phase conditions are as follows: the chromatographic column is a C18 chromatographic column, the length is 100mm, the diameter is 2.1mm, and the particle size of the filler is 1.7 mu m; the mobile phase consists of a mobile phase A and a mobile phase B, wherein the mobile phase A is a formic acid aqueous solution with the volume concentration of 0.1 percent, the mobile phase B is a formic acid acetonitrile solution with the volume concentration of 0.1 percent, the flow rate is 0.3mL/min, the column temperature is 40 ℃, and the gradient elution procedure is as follows: the volume fraction of the mobile phase B is changed from 5% to 30% in 0-5 min; 5-10min, the volume fraction of the mobile phase B is changed from 30% to 70%; the volume fraction of the mobile phase B is changed from 70% to 95% in 10-11 min; 11-12min, the volume fraction of the mobile phase B is kept 95%; 12-12.1min, the volume fraction of the mobile phase B is changed from 95% to 5%; 12.1-14min, and the volume fraction of the mobile phase B is kept 5%;
the mass spectrometry conditions were as follows: selecting an electrospray ion source in a positive and negative ion mode, wherein the parameters of the positive ion source include 250 ℃ of sheath gas temperature, 11L/min of sheath gas flow, 150 ℃ of drying gas, 15L/min of drying gas flow, 25psi of atomizer air pressure, 4000V of capillary tube voltage and 10-40eV of Collision Energy (CE); negative ion source parameters: the temperature of the sheath gas is 320 ℃, the flow rate of the sheath gas is 11L/min, the temperature of the drying gas is 150 ℃, the flow rate of the drying gas is 15L/min, the air pressure of the atomizer is 45psi, the voltage of the capillary tube is 3500V, and the Collision Energy (CE) is 10-40 eV.
The total ion flow diagram of the rosa roxburghii tratt water extract and the rosa roxburghii tratt concentrated solution obtained by the detection method of the embodiment is shown in figure 1.
Example 2
The embodiment provides a method for establishing a roxburgh rose ingredient database. The method for establishing the roxburgh rose ingredient database comprises the following steps of:
(S1) establishing a primary database of the roxburgh rose components: comparing the ion data of the concentrated solution of Rosa roxburghii Tratt obtained in example 1 with databases (HMDB, Pubchem and METLIN) and ion data in literature to identify its components, and supplementing and identifying components not reported in the above literature according to common general knowledge in the art in combination with Scifinder (scifider. cas. org /) database, and recording molecular formulas, relative retention times, parent ion and ion data, and reported efficacies of each identified component to obtain a primary database of Rosa roxburghii Tratt components;
(S2) expansion of the primary database of Rosa roxburghii Tratt components: library the LC-MS/MS data of the rosa roxburghii tratt aqueous extract obtained in example 1 was analyzed using the same process as the step (S1) to identify its components and expand the rosa roxburghii tratt component primary database to obtain a rosa roxburghii tratt component database (shown in table 1);
(S3) verification of the Rosa roxburghii Tratt ingredient database: the LC-MS/MS detection method in example 1 and the rosa roxburghii tratt ingredient database obtained in example 2 were used to perform mass detection on other rosa roxburghii tratt products to verify the applicability of the LC-MS/MS detection method and the rosa roxburghii tratt ingredient database, where the verification criteria were that the retention time, the primary mass spectrum data, and the secondary mass spectrum data of the ingredients in the identification result were consistent with the database (retention time ± 0.2min, compound-to-substance ratio (m/z) ± 50ppm), that the number of compounds in the identification result were more than 30% (i.e., 35) consistent with the database, or that the major ingredients such as flavone and small-molecule acid (relative molecular mass less than 500) were consistent with the database at a rate higher than 50%.
Other Rosa roxburghii products can be prepared by commercial Rosa roxburghii juice such as Rosa roxburghii natural high vitamin C beverage produced by health industry of Wangjie, Guangzhou, and the total ion flow diagram of the beverage is shown in FIG. 2; the total ion flow diagram of the raw roxburgh rose juice is shown in figure 3; the identification results of the obtained Citrobacter natural high-vitamin C beverage and the database are 72 compounds in total, and the identification results of the raw Rosa roxburghii juice and the database are 43 compounds in total, wherein the identification results of part of the components are shown in figure 4. The results show that the LC-MS/MS detection method in the embodiment 1 and the roxburgh rose component database established in the embodiment 2 have wide applicability, and can realize rapid and comprehensive component analysis and identification on commercial roxburgh rose juice and roxburgh rose raw juice;
(S4) presentation of the database: the verified database is combined with different use scenes and presented in the forms of WeChat small programs, web pages, H5 and the like, so that the database can be conveniently used by users.
The LC-MS/MS detection method in embodiment 1 and the rosa roxburghii tratt composition database established in embodiment 2 can quickly detect the change of rosa roxburghii tratt product components caused by the quality change of raw materials, the change of production process and other factors, and have an opportunity to be used for quality monitoring of rosa roxburghii tratt finished products and standardize the industrialized development of rosa roxburghii tratt.
TABLE 1 database
Figure BDA0003105785620000071
Figure BDA0003105785620000081
Figure BDA0003105785620000091
Figure BDA0003105785620000101
Figure BDA0003105785620000111
Figure BDA0003105785620000121
Figure BDA0003105785620000131
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. The method for detecting the components of the roxburgh rose sample is characterized by comprising the following steps of:
(1) processing a roxburgh rose sample to obtain a test sample solution;
(2) injecting the test solution into a liquid phase tandem mass spectrometer for detection;
wherein, the liquid phase conditions are as follows: the chromatographic column is a C18 chromatographic column, the mobile phase consists of a mobile phase A and a mobile phase B, the mobile phase A is formic acid aqueous solution with the volume concentration of 0.05-0.2%, the mobile phase B is formic acid acetonitrile solution with the volume concentration of 0.05-0.2%, gradient elution is carried out, the flow rate is 0.1-1 mL/min, and the column temperature is 30-50 ℃;
the mass spectrometry conditions were as follows: selecting an electrospray ion source, a positive and negative ion mode and positive ion source parameters: the temperature of the sheath gas is 240-260 ℃, the flow rate of the sheath gas is 10-12L/min, the temperature of the auxiliary gas is 140-160 ℃, the flow rate of the auxiliary gas is 14-16L/min, the air pressure of a sprayer is 23-27 psi, the voltage of a capillary tube is 3800-4200V, and the collision energy is 10-40 eV; negative ion source parameters: the temperature of the sheath gas is 310-330 ℃, the flow rate of the sheath gas is 10-12L/min, the temperature of the auxiliary gas is 140-160 ℃, the flow rate of the auxiliary gas is 14-16L/min, the air pressure of the sprayer is 43-47 psi, the voltage of the capillary tube is 3300-3700V, and the collision energy is 10-40 eV;
the roxburgh rose sample is roxburgh rose or a product thereof.
2. The detection method according to claim 1, wherein the gradient elution procedure is: the volume fraction of the mobile phase B is changed from 5% to 30% in 0-5 min; 5-10min, the volume fraction of the mobile phase B is changed from 30% to 70%; the volume fraction of the mobile phase B is changed from 70% to 95% in 10-11 min; 11-12min, the volume fraction of the mobile phase B is kept 95%; 12-12.1min, the volume fraction of the mobile phase B is changed from 95% to 5%; 12.1-14min, the volume fraction of mobile phase B is kept 5%.
3. The detection method according to claim 2, wherein the step (2) is carried out according to the following conditions of liquid phase and mass spectrum:
liquid phase: the mobile phase A is formic acid aqueous solution with volume concentration of 0.1 percent, and the mobile phase B is formic acid acetonitrile solution with volume concentration of 0.1 percent;
mass spectrometry positive ion source parameters: the temperature of the sheath gas is 250 ℃, the flow rate of the sheath gas is 11L/min, the temperature of the auxiliary gas is 150 ℃, the flow rate of the auxiliary gas is 15L/min, the air pressure of a sprayer is 25psi, the voltage of a capillary tube is 4000V, and the collision energy is 10-40 eV;
mass spectrum anion source parameters: the temperature of the sheath gas is 320 ℃, the flow rate of the sheath gas is 11L/min, the temperature of the auxiliary gas is 150 ℃, the flow rate of the auxiliary gas is 15L/min, the air pressure of the sprayer is 45psi, the voltage of the capillary tube is 3500V, and the collision energy is 10-40 eV.
4. The detection method according to claim 1, wherein the column has a length of 100mm, a diameter of 2.1mm, and a filler particle diameter of 1.7 μm.
5. The assay of claim 1, wherein the sample of Rosa roxburghii Tratt is Rosa roxburghii Tratt, Rosa roxburghii Tratt extract, Rosa roxburghii Tratt concentrate, or Rosa roxburghii Tratt juice.
6. The assay of claim 5, wherein the sample of Rosa roxburghii is Rosa roxburghii; the step (1) is as follows: juicing the whole roxburgh rose, and carrying out solid-liquid separation to obtain a solution, namely a test solution.
7. The assay of claim 5, wherein the sample of Rosa roxburghii is Rosa roxburghii; the step (1) is as follows: crushing Rosa roxburghii, extracting with water, collecting the extractive solution, concentrating, dissolving with acetonitrile water solution, and performing solid-liquid separation to obtain a sample solution.
8. The assay of claim 5, wherein the sample of Rosa roxburghii is Rosa roxburghii juice; the step (1) is as follows: and (3) carrying out solid-liquid separation on the roxburgh rose juice to obtain a solution, namely a test sample solution.
9. A method for establishing a roxburgh rose ingredient database is characterized by comprising the following steps:
(S1) testing the sample of rosa roxburghii tratt according to the testing method of any one of claims 1 to 7;
(S2) analyzing the LC-MS/MS data obtained in the step (S1) in combination with existing databases and literature to identify the components of the rosa roxburghii tratt sample, and recording molecular formulas, relative retention times, parent ions and ion data of each identified component to obtain a rosa roxburghii tratt component database.
10. The method of claim 8, further comprising the steps of:
detecting different roxburgh rose samples to verify the applicability of an LC-MS/MS method and a roxburgh rose component database;
and presenting the verified roxburgh rose component database for the user to use.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120148692A1 (en) * 2010-06-18 2012-06-14 Srm University Novel herbal formulation for the prevention and management of type-2 diabetes mellitus and vascular complications associated with diabetes
CN106153761A (en) * 2016-06-07 2016-11-23 贵州师范大学 The method of 3 kinds of flavones ingredients in detection seedless roxburgh rose fruit simultaneously
CN108896670A (en) * 2018-06-19 2018-11-27 陈溪 PPCPs pollutant rapid screening detection method in Drinking Water
CN109187840A (en) * 2018-11-08 2019-01-11 南京大学 The high flux examination analysis method of organic pollutant in a kind of blood
CN110196290A (en) * 2019-04-02 2019-09-03 贵州医科大学 Ellagic acid content assaying method in a kind of Rosa roxburghii Tratt

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120148692A1 (en) * 2010-06-18 2012-06-14 Srm University Novel herbal formulation for the prevention and management of type-2 diabetes mellitus and vascular complications associated with diabetes
CN106153761A (en) * 2016-06-07 2016-11-23 贵州师范大学 The method of 3 kinds of flavones ingredients in detection seedless roxburgh rose fruit simultaneously
CN108896670A (en) * 2018-06-19 2018-11-27 陈溪 PPCPs pollutant rapid screening detection method in Drinking Water
CN109187840A (en) * 2018-11-08 2019-01-11 南京大学 The high flux examination analysis method of organic pollutant in a kind of blood
CN110196290A (en) * 2019-04-02 2019-09-03 贵州医科大学 Ellagic acid content assaying method in a kind of Rosa roxburghii Tratt

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
MENG-HUA LIU ET AL: "Chemical Analysis of Dietary Constituents in Rosa roxburghii and Rosa sterilis Fruits", 《MOLECULES》 *
QIONG-QIONG YANG ET AL: "Phytochemicals, essential oils, and bioactivities of an underutilized wild fruit Cili (Rosa roxburghii)", 《INDUSTRIAL CROPS & PRODUCTS》 *
李剑豪 等: "UPLC-Q-TOF-MSE技术结合UNIFI筛查平台快速分析刺梨籽中化学成分", 《质谱学报》 *

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