CN113075347A - High performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol - Google Patents
High performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol Download PDFInfo
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- CN113075347A CN113075347A CN202110358172.6A CN202110358172A CN113075347A CN 113075347 A CN113075347 A CN 113075347A CN 202110358172 A CN202110358172 A CN 202110358172A CN 113075347 A CN113075347 A CN 113075347A
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Abstract
The invention discloses a high performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol, which is provided with a standard solution of 45 polyphenols, and comprises the following steps: respectively taking 10uL of the 45 kinds of polyphenol standard solution, mixing to obtain a mixed standard solution with the concentration of 0.021mg/mL, and diluting step by step; diluting the mixed standard solution to 1ppm, and respectively optimizing mass spectrum parameters; and (5) performing high performance liquid chromatography-mass spectrometry on the diluted mixed standard solution by using the mass spectrum parameters obtained by optimizing in the step S2, and finally obtaining a mass spectrogram of the sample to be detected. The method has the advantages of wide measuring range, high sensitivity and high efficiency, so that the qualitative and quantitative analysis can be rapidly carried out on the 43 polyphenols.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry and biochemistry, and particularly relates to a high performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol.
Technical Field
The polyphenol is an important secondary metabolite in a plant body, the polyphenol compound mainly comprises three components of phenolic acid, flavonoid and tannin, and the plant polyphenol not only can assist the plant to prevent the invasion of plant diseases and insect pests, but also has stronger antioxidant activity, can effectively reduce free radicals generated by oxidative stress, and reduces various chronic diseases caused by oxygen free radicals, such as cardiovascular and cerebrovascular diseases, cancer, obesity, Alzheimer disease, cataract, degenerative functional diseases and the like.
At present, the analytical detection methods of polyphenols include electrochemical methods, spectrophotometer methods, thin layer chromatography, High Performance Liquid Chromatography (HPLC) methods, and the like. The spectrophotometer method is mostly used for measuring the content of total phenols, and most of the existing methods for quantifying polyphenol components are high performance liquid chromatography, but the high performance liquid chromatography has low sensitivity and can quantify all components only when the components reach the separation degree.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a high performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a high performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapid detection of polyphenols, having a standard solution of 43 polyphenols, said method comprising the steps of:
s1, respectively taking 10uL of the 45 polyphenol standard solutions, mixing to obtain a mixed standard solution with the concentration of 0.021mg/mL, and diluting step by step;
s2, diluting the mixed standard solution to 1ppm, and respectively optimizing mass spectrum parameters;
s3, performing high performance liquid chromatography-mass spectrometry on the diluted mixed standard solution by using the mass spectrum parameters obtained by optimizing in the step S2, and finally obtaining a mass spectrum of the sample to be detected.
The mass spectrum parameters after optimization are CAD:4, CUR:30, GS1:55, GS2:55, IS:5500, TEM: 450, EP-10 and CXP-12.
The chromatographic conditions of the high performance liquid chromatograph are set as follows:
and (3) analyzing the column: f5, 2.1 × 100,2.6 μm;
mobile phase: ultra pure water (A), acetonitrile (B) and gradient elution;
flow rate: 0.1 mL/min;
detecting the temperature: 40 ℃;
sample introduction volume: 5 mu L of the solution;
elution mode (negative ion mode): gradient elution for 0min, wherein A: B is 90: 10; 15min, wherein A and B are 75: 25; 20min, wherein A and B are 70: 30; 32min, wherein A is 40: 60; 35min, wherein A and B are 95: 5; 38min, wherein A and B are 90: 10;
detection time: 38 min;
elution mode (positive ion mode): gradient elution for 0min, wherein A: B is 90: 10; 20min, wherein A is 40: 60; 25min, wherein A and B are 10 to 90; 28min, A: B: 5: 95; 29min, wherein A and B are 90: 10;
detection time: and 29 min.
It is to be noted that the present invention provides a high performance liquid chromatography detection method for simultaneously detecting 45 polyphenols, wherein the 45 polyphenols comprise 16 phenolic acids 3, 4-dihydroxybenzoic acid, salicylic acid, o-methylbenzoic acid, vanillic acid, gallic acid, pyrogallic acid, caffeic acid, syringic acid, sinapic acid, ferulic acid, trans-ferulic acid, 2-methoxycinnamic acid, 4, 6 dimethylamino cinnamaldehyde, trans-cinnamic acid, chlorogenic acid and p-coumaric acid; 2-coumarins 7-hydroxycoumarin and coumarin; 7-flavone-3-alcohol catechin, epicatechin, procyanidin B4, procyanidin B1, procyanidin B2, procyanidin A1, and procyanidin A2; 20 flavonoldihydroquercetin, quercetin, apigenin, quercetin-3-O-glucoside, myricetin, dihydromyricetin, myricetin-3-O-galactoside, kaempferol-glucoside, curcumin, kaempferol-3 ', 5' neohesperidin, kaempferol-3-O-rutinoside, quercetin-3-O-rutinoside-7-O-rhamnose, kaempferol, naringin, hesperidin, naringenin, luteolin, narcissus, typhanin, and rutin.
The method has the advantages of wide measuring range, high sensitivity and high efficiency, so that the qualitative and quantitative analysis can be rapidly carried out on the 45 polyphenols.
Drawings
FIG. 1 shows the results of a portion of 45 assays performed using the method of the invention;
FIG. 2 shows the results of the detection of another part of 45 samples by the method of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention will be further described with reference to the accompanying drawings, and it should be noted that the present embodiment is based on the technical solution, and the detailed implementation and the specific operation process are provided, but the protection scope of the present invention is not limited to the present embodiment.
Examples
The invention relates to a high performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol, which is a standard solution with 43 kinds of polyphenol, and the method comprises the following steps:
s1, respectively taking 10uL of the 45 polyphenol standard solutions, mixing to obtain a mixed standard solution with the concentration of 0.021mg/mL, and diluting step by step;
s2, diluting the mixed standard solution to 1ppm, and respectively optimizing mass spectrum parameters;
s3, performing high performance liquid chromatography-mass spectrometry on the diluted mixed standard solution by using the mass spectrum parameters obtained by optimizing in the step S2, and finally obtaining a mass spectrum of the sample to be detected.
The mass spectrum parameters after optimization are CAD:4, CUR:30, GS1:55, GS2:55, IS:5500, TEM: 450, EP-10 and CXP-12.
The chromatographic conditions of the high performance liquid chromatograph are set as follows:
and (3) analyzing the column: f5, 2.1 × 100,2.6 μm;
mobile phase: ultra pure water (A), acetonitrile (B) and gradient elution;
flow rate: 0.1 mL/min;
detecting the temperature: 40 ℃;
sample introduction volume: 5 mu L of the solution;
elution mode (negative ion mode): gradient elution for 0min, wherein A: B is 90: 10; 15min, wherein A and B are 75: 25; 20min, wherein A and B are 70: 30; 32min, wherein A is 40: 60; 35min, wherein A and B are 95: 5; 38min, wherein A and B are 90: 10;
detection time: 38 min;
elution mode (positive ion mode): gradient elution for 0min, wherein A: B is 90: 10; 20min, wherein A is 40: 60; 25min, wherein A and B are 10 to 90; 28min, A: B: 5: 95; 29min, wherein A and B are 90: 10;
detection time: and 29 min.
For the detection of 45 polyphenols in the invention, the selected reaction monitoring parent ions, daughter ions and collision energy are shown in table 2.
Further, the results of the detection of the 45 polyphenol mixed solution of the present invention are shown in fig. 1 and 2. Therefore, the method has the characteristics of wide measurement range, high sensitivity and high efficiency, so that the qualitative and quantitative analysis can be rapidly carried out on the 45 polyphenols.
Various modifications may be made by those skilled in the art based on the above teachings and concepts, and all such modifications are intended to be included within the scope of the present invention as defined in the appended claims.
Claims (3)
1. A high performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol is provided, wherein the method comprises a standard solution with 43 polyphenols, and is characterized by comprising the following steps:
s1, respectively taking 10uL of the 45 polyphenol standard solutions, mixing to obtain a mixed standard solution with the concentration of 0.021mg/mL, and diluting step by step;
s2, diluting the mixed standard solution to 1ppm, and respectively optimizing mass spectrum parameters;
s3, performing high performance liquid chromatography-mass spectrometry on the diluted mixed standard solution by using the mass spectrum parameters obtained by optimizing in the step S2, and finally obtaining a mass spectrum of the sample to be detected.
2. The high performance liquid chromatography-triple quadrupole mass spectrometry combination method for rapidly detecting polyphenol according to claim 1, wherein the optimized mass spectrometry parameters are CAD:4, CUR:30, GS1:55, GS2:55, IS:5500, TEM: 450, EP-10 and CXP-12.
3. The method for rapidly detecting polyphenols according to claim 1, wherein the chromatographic conditions of the high performance liquid chromatograph are set as follows:
and (3) analyzing the column: f5, 2.1 × 100,2.6 μm;
mobile phase: ultra pure water (A), acetonitrile (B) and gradient elution;
flow rate: 0.1 mL/min;
detecting the temperature: 40 ℃;
sample introduction volume: 5 mu L of the solution;
elution mode (negative ion mode): gradient elution for 0min, wherein A: B is 90: 10; 15min, wherein A and B are 75: 25; 20min, wherein A and B are 70: 30; 32min, wherein A is 40: 60; 35min, wherein A and B are 95: 5; 38min, wherein A and B are 90: 10;
detection time: 38 min;
elution mode (positive ion mode): gradient elution for 0min, wherein A: B is 90: 10; 20min, wherein A is 40: 60; 25min, wherein A and B are 10 to 90; 28min, A: B: 5: 95; 29min, wherein A and B are 90: 10;
detection time: and 29 min.
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Cited By (2)
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| CN114577938A (en) * | 2022-03-03 | 2022-06-03 | 江南大学 | HPLC detection method for simultaneously determining seven phenols content in pine pollen extract |
| CN114740100A (en) * | 2022-03-10 | 2022-07-12 | 西北农林科技大学 | LC-MS/MS detection method of gallotannin in plant |
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Cited By (3)
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| CN114577938A (en) * | 2022-03-03 | 2022-06-03 | 江南大学 | HPLC detection method for simultaneously determining seven phenols content in pine pollen extract |
| CN114740100A (en) * | 2022-03-10 | 2022-07-12 | 西北农林科技大学 | LC-MS/MS detection method of gallotannin in plant |
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