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CN110988245A - Method for rapidly detecting content of vitamin E in vegetable oil and fat and analogues thereof by ultra-high performance combined phase chromatography-mass spectrometry - Google Patents

Method for rapidly detecting content of vitamin E in vegetable oil and fat and analogues thereof by ultra-high performance combined phase chromatography-mass spectrometry Download PDF

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CN110988245A
CN110988245A CN201911355790.4A CN201911355790A CN110988245A CN 110988245 A CN110988245 A CN 110988245A CN 201911355790 A CN201911355790 A CN 201911355790A CN 110988245 A CN110988245 A CN 110988245A
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vitamin
vegetable oil
tocopherol
mass spectrometry
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张榴萍
周洲
罗世龙
鲍鏖天
钱国平
谢军
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Sinograin Zhenjiang Grain And Oil Quality Inspection Center Co ltd
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    • 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
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • 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
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    • G01N30/04Preparation or injection of sample to be analysed
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    • 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
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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Abstract

The invention discloses a method for rapidly detecting the content of vitamin E in vegetable oil and analogues thereof by an ultra-efficient combined phase chromatography-mass spectrometry, which comprises the following specific steps: dissolving vegetable oil or vegetable oil analogue in isooctane or normal hexane to obtain a sample solution to be detected; separating four vitamin E isomers by ultra-high performance combined chromatography, and detecting the concentrations of the four vitamin E isomers in a sample solution to be detected by quadrupole mass spectrometry; calculating to obtain the content of vitamin E isomer in the vegetable oil or the vegetable oil analogue; the method can realize the rapid separation of the four vitamin E isomers and quantitatively detect the content of the four vitamin E isomers in the vegetable oil or vegetable oil analogues, and has the advantages of high analysis speed, strong anti-interference capability, high sensitivity and the like.

Description

Method for rapidly detecting content of vitamin E in vegetable oil and fat and analogues thereof by ultra-high performance combined phase chromatography-mass spectrometry
Technical Field
The invention particularly relates to a method for rapidly detecting the content of vitamin E in vegetable oil and analogues thereof by an ultra-efficient combined phase chromatography-mass spectrometry method.
Background
The α -tocopherol is most easily absorbed and utilized by human body and has the highest physiological activity, and other types of vitamin E also play very important roles in human body.
Natural vitamin E is a collective term for a variety of fat-soluble tocopherols and tocotrienols produced by plant photosynthesis. Human beings cannot synthesize vitamin E by themselves and can only ingest it through food, and about 70% of this is derived from vegetable fats and oils. The content and composition of vitamin E in different vegetable oil are different.
The method for detecting the content of the vitamin E comprises various methods such as a titration method, an electrochemical analysis method, a spectroscopic method, a chromatography-mass spectrometry combined method and the like, wherein the titration method, the electrochemical analysis method and the spectroscopic method are only limited to measuring a certain isomer or total amount of the vitamin E and are easily interfered by a sample matrix, the chromatographic method is difficult to effectively separate the isomer β -tocopherol and gamma-tocopherol, and the reverse phase chromatography of a special filler chromatographic column and the normal phase chromatography of a silica gel chromatographic column can realize the separation of β -tocopherol and gamma-tocopherol under certain chromatographic conditions, but the separation time is long and the consumption of an organic solvent is large.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for rapidly detecting the content of vitamin E in vegetable oil and analogues thereof by an ultra-high performance synthesis phase chromatography-mass spectrometry, which can rapidly separate α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol isomers in the vegetable oil and has the advantages of high separation speed, strong anti-interference capability, high sensitivity and the like.
The technical scheme for solving the problems comprises the following steps: a method for rapidly detecting the content of vitamin E in vegetable oil and fat and analogues thereof by an ultra-high performance coherent chromatography-mass spectrometry method comprises the following steps:
preparing raw materials in step (1): weighing vegetable oil or vegetable oil analogue 0.01-0.5g, extracting solvent 10-30ml, and antioxidant 0.005-0.05 g;
preparing a sample solution to be detected: placing vegetable oil or vegetable oil analogue, extraction solvent and antioxidant in a glass beaker for ultrasonic dissolution to obtain a mixture A; transferring the mixture A into a 100ml brown volumetric flask, fixing the volume to a scale by using an extraction solvent, carrying out vortex oscillation and uniform mixing, and filtering by using an organic phase filter membrane to obtain a sample solution to be detected;
preparing standard series working solutions in step (3), namely preparing α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol standard substances into standard series working solutions with different concentrations;
determining standard series working solutions and drawing a standard curve, namely determining peak areas of α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol four vitamin E isomers in the standard series working solutions by adopting an ultra-performance convergence chromatography-mass spectrometry method, and calculating a linear regression equation by taking the peak areas of the four vitamin E isomers as a vertical coordinate and the concentration as a horizontal coordinate;
and (5) determining the sample liquid to be detected, namely determining peak areas of α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol four vitamin E isomers in the sample liquid to be detected by adopting an ultra-high performance convergence chromatography-mass spectrometry method under the same detection condition as that in the step (4), calculating the concentration rho by adopting an external standard method through the standard curve, and respectively calculating the content of the four vitamin E isomers in the vegetable oil or the vegetable oil analogue through a formula (rho multiplied by V)/m.
Further, the vegetable oil is corn oil, sunflower seed oil, soybean oil and rapeseed oil.
Further, the vegetable oil and fat analogue is a corn oil deodorized distillate, a sunflower oil deodorized distillate, a soybean oil deodorized distillate, a rapeseed oil deodorized distillate.
Further, the extraction solvent is isooctane or n-hexane.
Further, the ultrasonic dissolving time is 2-5 min.
Further, the pore size of the organic phase filter membrane is 0.22 μm.
Furthermore, in the methanol-isopropanol mixed solution, the volume fraction of isopropanol is 0-30%.
Further, in the step (4) and the step (5), the detection conditions of the ultra-high performance phase-compatible chromatography are as follows: AcquisetUPC 2TM BEH column was used, column parameters: the inner diameter of the column is 3mm, the length of the column is 100mm, and the grain diameter of the filler is 1.7 mu m; the column temperature is 50-70 ℃, and the system back pressure is 1800 plus 2000 psi; taking supercritical carbon dioxide and methanol-isopropanol mixed solution as a mobile phase;
the elution gradient was: 0-1.5 min: 98% -95% of supercritical carbon dioxide, 1.5-1.8 min: 95% -80% of supercritical carbon dioxide, 1.8-2.0 min: 80% -98% of supercritical carbon dioxide, 2.0-2.5 min: 98% supercritical carbon dioxide; sample introduction amount: 1-5 μ L; flow rate: 1.5-3 ml/min.
Further, in the step (4) and the step (5), the mass spectrometry detection conditions are as follows: an electrospray ion source; a positive ion mode; the air pressure of the air curtain is 25-40 psi; ionization voltage 4500-; the pressure of the atomization gas is 40-50 psi; auxiliary heating gas pressure 40-60 psi; the ion source temperature is 450 ℃ and 550 ℃; the compensation solvent is methanol; single ion monitoring scan mode or multiple reaction monitoring scan mode.
Furthermore, the flow rate of the compensation solvent is 0.2-0.3ml/min, and the compensation solvent contains 0.1% -1% of formic acid by volume fraction.
The invention has the following beneficial effects:
(1) according to the invention, the sample to be detected is obtained by directly dissolving the sample with the extraction solvent, and four vitamin E isomers are rapidly and effectively separated by optimizing chromatographic conditions, so that the detection time is greatly shortened.
(2) The method can quickly and effectively separate four vitamin E isomers by optimizing chromatographic conditions, and is suitable for both single quadrupole mass spectrometry and triple quadrupole mass spectrometry.
(3) According to the invention, by optimizing the mass spectrum conditions, the response of four vitamin E isomers on the quadrupole mass spectrum is improved, and the detection sensitivity is improved.
(4) The invention increases the constant volume of the sample liquid to be measured, reduces the sample volume, basically eliminates the matrix interference and improves the recovery rate of four vitamin E isomers by reducing the sample weighing amount of the vegetable oil or the vegetable oil analogue.
Drawings
FIG. 1 is an ion flow diagram of four vitamin E isomers in a sample solution to be tested in example 1 of the present invention;
FIG. 2 is an ion flow diagram of four vitamin E isomers in a sample solution to be tested in example 2 of the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1
A method for rapidly detecting the content of vitamin E in vegetable oil and fat and analogues thereof by an ultra-high performance coherent chromatography-mass spectrometry method comprises the following steps:
preparing raw materials in step (1): weighing 0.25g of corn oil, 30ml of isooctane and 0.010g of 2, 6-di-tert-butyl-p-cresol;
preparing a sample solution to be detected: placing the corn oil, isooctane and 2, 6-di-tert-butyl-p-cresol in a glass beaker, and ultrasonically dissolving for 2min to obtain a mixture A; transferring the mixture A into a 100ml brown volumetric flask, fixing the volume to the scale by using an extraction solvent, carrying out vortex oscillation and uniform mixing, and filtering by using an organic phase filter membrane with the aperture of 0.22 mu m to obtain a sample solution to be detected;
preparing standard series working solutions in step (3), namely preparing α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol standard substances into standard series working solutions with different concentrations;
determining standard series working solutions and drawing a standard curve, namely determining peak areas of α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol four vitamin E isomers in the standard series working solutions by adopting an ultra-performance convergence chromatography-mass spectrometry method, and calculating a linear regression equation by taking the peak areas of the four vitamin E isomers as a vertical coordinate and the concentration as a horizontal coordinate;
the ultra-high performance phase-matching chromatographic conditions are as follows: using Acquity UPC2TM BEH chromatography column, column parameters: the inner diameter of the column is 3mm, the length of the column is 100mm, and the grain diameter of the filler is 1.7 mu m; the column temperature is 50 ℃, and the system back pressure is 1800 psi; supercritical carbon dioxide and methanol-isopropanol mixed solution are used as mobile phase, and the volume fraction of isopropanol in the methanol-isopropanol mixed solution is 10%;
the elution gradient was: 0-1.5 min: 98% -95% of supercritical carbon dioxide, 1.5-1.8 min: 95% -80% of supercritical carbon dioxide, 1.8-2.0 min: 80% -98% of supercritical carbon dioxide, 2.0-2.5 min: 98% supercritical carbon dioxide; sample introduction amount: 1 mu L of the solution; flow rate: 1.8 ml/min;
the mass spectrum detection conditions are as follows: an electrospray ion source; a positive ion mode; air curtain pressure 35 psi; ionization voltage 5000V; atomizing gas pressure 45 psi; auxiliary heating gas pressure 50 psi; the ion source temperature is 500 ℃; the compensation solvent was 0.3ml/min methanol containing 0.1% formic acid, single ion monitoring scan mode.
TABLE 1 Mass Spectrometry parameters and monitoring ions
Analyte Molecular formula Monitoring ions tR/min DP
α -tocopherol C29H50O2 431.7 0.842 125
β -tocopherol C28H48O2 417.7 1.142 95
Gamma-tocopherol C28H48O2 417.7 1.229 95
Delta-tocopherol C27H46O2 403.7 1.423 130
And (5) measuring sample liquid to be measured, namely measuring peak areas of α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol four vitamin E isomers in the sample liquid to be measured under the same detection condition as that in the step (4), calculating the concentrations rho of the four vitamin E isomers in the sample liquid to be measured by adopting an external standard method through a standard curve in a table 2 and an ion flow diagram in a figure 1, and calculating the contents of the four vitamin E isomers in the corn oil shown in a table 3 through a formula (rho multiplied by V)/m respectively.
TABLE 2 Linear regression equation and related parameters for four vitamin E isomers
Figure BDA0002335882010000061
Note: the concentration of the x-vitamin E isomer; peak area of y-vitamin E isomer; detection limit-concentration at which the signal-to-noise ratio (S/N) is 3; quantitation limit-concentration at a signal-to-noise ratio (S/N) of 10.
As can be seen from Table 2, R of the linear regression equation2All are above 0.9990, and the standard curves of the four vitamin E isomers have good linear relation in corresponding concentration ranges.
TABLE 3 content of four vitamin E isomers in corn oil
Figure BDA0002335882010000062
Note: RSD-relative standard deviation.
For the results obtained in Table 3, recovery tests were performed by adding different concentrations of the four vitamin E isomers to the same corn oil. The results of the recovery test are shown in table 4, and it can be seen from table 4 that the recovery rates of the four vitamin E isomers were between 93% and 98%, and the recovery rates were good.
TABLE 4 recovery test
Figure BDA0002335882010000071
Example 2
A method for rapidly detecting the content of vitamin E in vegetable oil and fat and analogues thereof by an ultra-high performance coherent chromatography-mass spectrometry method comprises the following steps:
preparing raw materials in step (1): weighing 0.50g of sunflower seed oil, 20ml of n-hexane and 0.020g of tert-butylhydroquinone;
preparing a sample solution to be detected: placing sunflower seed oil, n-hexane and tert-butylhydroquinone in a glass beaker, and ultrasonically dissolving for 3min to obtain a mixture A; transferring the mixture A into a 100ml brown volumetric flask, fixing the volume to the scale by using an extraction solvent, carrying out vortex oscillation and uniform mixing, and filtering by using an organic phase filter membrane with the aperture of 0.22 mu m to obtain a sample solution to be detected;
preparing standard series working solutions in step (3), namely preparing α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol standard substances into standard series working solutions with different concentrations;
determining standard series working solutions and drawing a standard curve, namely determining peak areas of α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol four vitamin E isomers in the standard series working solutions by adopting an ultra-performance convergence chromatography-mass spectrometry method, and calculating a linear regression equation by taking the peak areas of the four vitamin E isomers as a vertical coordinate and the concentration as a horizontal coordinate;
the ultra-high performance phase-matching chromatographic conditions are as follows: adopting an Acquity UPC2TM BEH chromatographic column, wherein the inner diameter of the column is 3mm, the length of the column is 100mm, and the particle size of a filler is 1.7 mu m; the column temperature is 60 ℃, and the system back pressure is 1900 psi; supercritical carbon dioxide and methanol-isopropanol mixed solution are used as mobile phase, and the volume fraction of isopropanol in the methanol-isopropanol mixed solution is 5%;
the elution gradient was: 0-1.5 min: 98% -95% of supercritical carbon dioxide, 1.5-1.8 min: 95% -80% of supercritical carbon dioxide, 1.8-2.0 min: 80% -98% of supercritical carbon dioxide, 2.0-2.5 min: 98% supercritical carbon dioxide; sample introduction amount: 1 mu L of the solution; flow rate: 1.8 ml/min;
the mass spectrum detection conditions are as follows: an electrospray ion source; a positive ion mode; air curtain pressure 40 psi; ionization voltage 4500V; the atomization gas pressure is 50 psi; auxiliary heating gas pressure 50 psi; the ion source temperature is 500 ℃; the compensation solvent is 0.2ml/min methanol, and the methanol contains 0.1 percent of formic acid by volume fraction; multiple reaction monitoring scan mode.
TABLE 5 Mass Spectrometry parameters and monitoring ions are shown in the Table
Figure BDA0002335882010000081
And (5) determining a sample solution to be detected, namely determining peak areas of α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol isomers in the sample solution to be detected under the same detection condition as that in the step (4), calculating the concentrations rho of the four vitamin E isomers in the sample solution to be detected by adopting an external standard method through a standard curve in a table 6 and an ion flow diagram in a figure 2, and respectively calculating the contents of the four vitamin E isomers in the sunflower seed oil shown in a table 7 through a formula (rho multiplied by V)/m.
TABLE 6 Linear regression equation and related parameters for four vitamin E isomers
Figure BDA0002335882010000091
Note: the concentration of the x-vitamin E isomer; peak area of y-vitamin E isomer; detection limit-concentration at which the signal-to-noise ratio (S/N) is 3; quantitation limit-concentration at a signal-to-noise ratio (S/N) of 10.
As can be seen from Table 6, R of the linear regression equation2All are above 0.9990, and the standard curves of the four vitamin E isomers have good linear relation in corresponding concentration ranges.
TABLE 7 content of four vitamin E isomers in sunflower seed oil
Figure BDA0002335882010000092
Note: RSD-relative standard deviation.
For the detection results obtained in table 7, four vitamin E isomers at different concentrations were added to the same sunflower seed oil for recovery tests. The results of the recovery test are shown in table 8, and it can be seen from table 8 that the recovery rates of the four vitamin E isomers were between 90% and 98%, and the recovery rates were good.
TABLE 8 recovery test
Figure BDA0002335882010000101
Many other changes and modifications can be made without departing from the spirit and scope of the invention. It is to be understood that the invention is not to be limited to the specific embodiments, but only by the scope of the appended claims.

Claims (11)

1. A method for rapidly detecting the content of vitamin E in vegetable oil and fat and analogues thereof by an ultra-high performance coherent chromatography-mass spectrometry method is characterized by comprising the following steps:
preparing raw materials in step (1): weighing vegetable oil or vegetable oil analogue 0.01-0.5g, extracting solvent 10-30ml, and antioxidant 0.005-0.05 g;
preparing a sample solution to be detected: placing vegetable oil or vegetable oil analogue, extraction solvent and antioxidant in a glass beaker for ultrasonic dissolution to obtain a mixture A; transferring the mixture A into a brown volumetric flask of 100m l, fixing the volume to a scale by using an extraction solvent, carrying out vortex oscillation and uniform mixing, and filtering by using an organic phase filter membrane to obtain a sample solution to be detected;
preparing standard series working solutions in step (3), namely preparing α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol standard substances into standard series working solutions with different concentrations;
determining standard series working solutions and drawing a standard curve, namely determining peak areas of α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol four vitamin E isomers in the standard series working solutions by adopting an ultra-performance convergence chromatography-mass spectrometry method, and calculating a linear regression equation by taking the peak areas of the four vitamin E isomers as a vertical coordinate and the concentration as a horizontal coordinate;
and (5) determining the sample liquid to be detected, namely determining peak areas of α -tocopherol, β -tocopherol, gamma-tocopherol and delta-tocopherol four vitamin E isomers in the sample liquid to be detected by adopting an ultra-high performance convergence chromatography-mass spectrometry method under the same detection condition as that in the step (4), calculating the concentration rho by adopting an external standard method through the standard curve, and respectively calculating the content of the four vitamin E isomers in the vegetable oil or the vegetable oil analogue through a formula (rho multiplied by V)/m.
2. The method for rapidly detecting vitamin E content in vegetable oil and fat and analogues thereof according to claim 1, wherein the vegetable oil and fat is corn oil, sunflower seed oil, soybean oil or rapeseed oil.
3. The method for rapidly detecting vitamin E content in vegetable oil and fat and analogues thereof according to claim 1, wherein the vegetable oil and fat analogues are corn oil deodorized distillate, sunflower oil deodorized distillate, soybean oil deodorized distillate, rapeseed oil deodorized distillate.
4. The method for rapidly detecting the vitamin E content in vegetable oil and fat and analogues thereof by using the ultra-high performance chromatography-mass spectrometry as claimed in claim 1, wherein the extraction solvent is isooctane or n-hexane.
5. The method for rapidly detecting the vitamin E content in the vegetable oil and the analogues thereof by the ultra-high performance convergence chromatography-mass spectrometry as claimed in claim 1, wherein the antioxidant is 2, 6-di-tert-butyl-p-cresol and tert-butyl-hydroquinone.
6. The method for rapidly detecting the vitamin E content in the vegetable oil and fat and the analogues thereof by the ultra-high performance convergence chromatography-mass spectrometry as claimed in claim 1, wherein the ultrasonic dissolution time is 2-5 min.
7. The method for rapidly detecting the vitamin E content in the vegetable oil and the analogues thereof by the ultra-high performance combined chromatography-mass spectrometry as claimed in claim 1, wherein the volume fraction of the isopropanol in the methanol-isopropanol mixed solution is 0% -30%.
8. The method for rapidly detecting the content of vitamin E in vegetable fat and oil and analogues thereof by using the ultra-high performance phase-combining chromatography mass spectrometry as claimed in claim 1, 2, 3, 4, 5, 6 or 7, wherein in the step (4) and the step (5), the ultra-high performance phase-combining chromatography detection conditions are as follows: using Acquity UPC2TM BEH chromatography column, column parameters: the inner diameter of the column is 3mm, the length of the column is 100mm, and the grain diameter of the filler is 1.7 mu m; the column temperature is 50-70 ℃, and the system back pressure is 1800 plus 2000 psi; taking supercritical carbon dioxide and methanol-isopropanol mixed solution as a mobile phase;
the elution gradient was: 0-1.5 min: 98% -95% of supercritical carbon dioxide, 1.5-1.8 min: 95% -80% of supercritical carbon dioxide, 1.8-2.0 min: 80% -98% of supercritical carbon dioxide, 2.0-2.5 min: 98% supercritical carbon dioxide; sample introduction amount: 1-5 μ L; flow rate: 1.5-3 ml/min.
9. The method for rapidly detecting the content of vitamin E in vegetable fat and oil and analogues thereof by using the ultra-high performance phase-compatible chromatography-mass spectrometry as claimed in claim 1, 2, 3, 4, 5, 6 or 7, wherein in the step (4) and the step (5), the mass spectrometry detection conditions are as follows: an electrospray ion source; a positive ion mode; the air pressure of the air curtain is 25-40 psi; ionization voltage 4500-; the pressure of the atomization gas is 40-50 psi; auxiliary heating gas pressure 40-60 psi; the ion source temperature is 450 ℃ and 550 ℃; the compensation solvent is methanol; single ion monitoring scan mode or multiple reaction monitoring scan mode.
10. The method for rapidly detecting the vitamin E content in the vegetable oil and fat and the analogues thereof by the ultra-high performance convergence chromatography-mass spectrometry method as claimed in claim 8, wherein in the step (4) and the step (5), the mass spectrometry detection conditions are as follows: an electrospray ion source; a positive ion mode; the air pressure of the air curtain is 25-40 psi; ionization voltage 4500-; the pressure of the atomization gas is 40-50 psi; auxiliary heating gas pressure 40-60 psi; the ion source temperature is 450 ℃ and 550 ℃; the compensation solvent is methanol; single ion monitoring scan mode or multiple reaction monitoring scan mode.
11. The method for rapidly detecting the vitamin E content in the vegetable oil and the analogues thereof by the ultra-high performance phase-combination chromatography-mass spectrometry as claimed in claim 9, wherein the flow rate of the compensation solvent is 0.2-0.3ml/min, and the compensation solvent contains 0.1% -1% of formic acid by volume fraction.
CN201911355790.4A 2019-12-25 2019-12-25 Method for rapidly detecting content of vitamin E in vegetable oil and fat and analogues thereof by ultra-high performance combined phase chromatography-mass spectrometry Pending CN110988245A (en)

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CN113009041A (en) * 2021-03-16 2021-06-22 品测(上海)检测科技有限公司 Method for simultaneously determining eight vitamin E isomers in vegetable oil
WO2021217442A1 (en) * 2020-04-27 2021-11-04 深圳波顿香料有限公司 Convergence chromatography analysis method for tocopherol acetate in e-liquid
CN115078559A (en) * 2022-03-24 2022-09-20 杭州佰辰医学检验所有限公司 Rapid vitamin D detection method based on single quadrupole mass spectrometry, kit and application
CN115266999A (en) * 2022-08-05 2022-11-01 陇南市祥宇油橄榄开发有限责任公司 Qualitative and quantitative detection method for gamma-oryzanol in vegetable oil

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102435700A (en) * 2011-09-22 2012-05-02 明一(福建)婴幼儿营养品有限公司 Method for determining vitamin ADE content in infant food and dairy products
CN103399100A (en) * 2013-08-13 2013-11-20 中国热带农业科学院农产品加工研究所 Measuring method of vitamin E content in fruits
CN104914182A (en) * 2015-05-29 2015-09-16 安徽古井贡酒股份有限公司 Method for rapidly detecting four vitamins E in white spirit simultaneously by utilizing ultra performanceconvergence chromatography
CN105067733A (en) * 2015-07-16 2015-11-18 中国热带农业科学院农产品加工研究所 Method for measuring content of vitamin E in food with ultra-performance convergence chromatography

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102435700A (en) * 2011-09-22 2012-05-02 明一(福建)婴幼儿营养品有限公司 Method for determining vitamin ADE content in infant food and dairy products
CN103399100A (en) * 2013-08-13 2013-11-20 中国热带农业科学院农产品加工研究所 Measuring method of vitamin E content in fruits
CN104914182A (en) * 2015-05-29 2015-09-16 安徽古井贡酒股份有限公司 Method for rapidly detecting four vitamins E in white spirit simultaneously by utilizing ultra performanceconvergence chromatography
CN105067733A (en) * 2015-07-16 2015-11-18 中国热带农业科学院农产品加工研究所 Method for measuring content of vitamin E in food with ultra-performance convergence chromatography

Non-Patent Citations (7)

* Cited by examiner, † Cited by third party
Title
ANDREW AUBIN: "使用超高效合相色谱(UPC2)进行脂溶性维生素胶囊分析", 《WWW.WATERS.COM》 *
KATARZYNA TYSKIEWICZ ET AL: "Supercritical Fluid Chromatography with Photodiode Array Detection in the Determination of Fat-Soluble Vitamins in Hemp Seed Oil and Waste Fish Oil", 《MOLECULES》 *
LUCIE NOVÁKOVÁ ET AL: "The Benefits of Ultra-High-Performance Supercritical Fluid Chromatography in Determination of Lipophilic Vitamins in Dietary Supplements", 《CHROMATOGRAPHIA》 *
TAKASHI YARITA ET AL: "Supercritical fluid chromatographic determination of tocopherols on an ODS-silica gel column", 《JOURNAL OF CHROMATOGRAPHY A》 *
王春天 等: "同时分离九种脂溶性维生素的UPC~2方法", 《甘肃农业》 *
蒋崇文 等: "超临界流体色谱法分析天然维生素E", 《粮食与油脂》 *
郑熠斌 等: "正相高效液相色谱法测定食物中8种维生素E异构体及维生素A", 《色谱》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021217442A1 (en) * 2020-04-27 2021-11-04 深圳波顿香料有限公司 Convergence chromatography analysis method for tocopherol acetate in e-liquid
CN113009041A (en) * 2021-03-16 2021-06-22 品测(上海)检测科技有限公司 Method for simultaneously determining eight vitamin E isomers in vegetable oil
CN113009041B (en) * 2021-03-16 2023-01-06 品测(上海)检测科技有限公司 Method for simultaneously determining eight vitamin E isomers in vegetable oil
CN115078559A (en) * 2022-03-24 2022-09-20 杭州佰辰医学检验所有限公司 Rapid vitamin D detection method based on single quadrupole mass spectrometry, kit and application
CN115078559B (en) * 2022-03-24 2024-05-28 杭州佰辰医学检验所有限公司 Vitamin D rapid detection method based on single quadrupole mass spectrometry, kit and application
CN115266999A (en) * 2022-08-05 2022-11-01 陇南市祥宇油橄榄开发有限责任公司 Qualitative and quantitative detection method for gamma-oryzanol in vegetable oil
CN115266999B (en) * 2022-08-05 2024-06-18 陇南市祥宇油橄榄开发有限责任公司 Qualitative and quantitative detection method for gamma-oryzanol in vegetable oil

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