CN113376285A - Liquid chromatography for determining vitamin B12 addition in infant food and milk - Google Patents

Liquid chromatography for determining vitamin B12 addition in infant food and milk Download PDF

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CN113376285A
CN113376285A CN202110656055.8A CN202110656055A CN113376285A CN 113376285 A CN113376285 A CN 113376285A CN 202110656055 A CN202110656055 A CN 202110656055A CN 113376285 A CN113376285 A CN 113376285A
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vitamin
solution
liquid chromatography
infant food
determining
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李清伟
周慧
卢垣宇
周筑萍
任沁怡
徐显松
张英姿
田义霞
李本良
卢霞
宋忠霞
王业钤
杨丽
曹天顺
刘晶晶
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Guizhou Product Quality Inspection And Testing Institute
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    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0006—Organic membrane manufacture by chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/14—Preparation by elimination of some components
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating 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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    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
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    • G01N30/14—Preparation by elimination of some components
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    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • G01N2030/3007—Control of physical parameters of the fluid carrier of temperature same temperature for whole column
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Abstract

The invention belongs to the technical field of food nutrition detection, and discloses a liquid chromatography for determining the addition of vitamin B12 in infant food and dairy products, which comprises the following steps: adding a proper amount of sterilized water into infant food and dairy products to be measured, and uniformly stirring to obtain liquid to be measured; filtering and sterilizing the obtained liquid to be measured by utilizing a pre-prepared nanofiber filtering membrane to obtain the liquid to be measured after filtering and sterilizing; b12 standard working solution is prepared; establishing a standard working curve: analyzing based on the prepared B12 standard stock solution, and establishing a standard working curve; detecting the content of vitamin B12 in the solution to be detected by liquid chromatography; and determining the addition amount of the vitamin B12 in the infant food and the dairy product according to the established standard working curve and the detection result of the solution to be detected. The detection method has high detection accuracy and good repeatability, and can meet the requirements of qualitative and quantitative vitamin detection.

Description

Liquid chromatography for determining vitamin B12 addition in infant food and milk
Technical Field
The invention belongs to the technical field of food nutrition detection, and particularly relates to a liquid chromatography for determining the addition of vitamin B12 in infant food and dairy products.
Background
At present: vitamins can be divided into two categories, fat-soluble vitamins including vitamin A, D, E, K and water-soluble vitamins including vitamin B group and vitamin C. They are micronutrients required by the organism, and generally cannot be produced by the organism itself, and need to be obtained by means of diet and the like. The normal people need to take 2500-3000 international units of vitamin A and 300-400 international units of vitamin D every day. If the organism lacks vitamins, the immunity is reduced, and the disease is easy to suffer.
Infant rice flour is recommended to be added for infants more than 6 months old, and has great market demand in China. The third quarter spot check result of 2012 of the national quality control bureau shows that the sampling qualification rate of the infant rice flour product is only 54.2%, and the centralized problem is represented by no addition of a nutrition enhancer or insufficient nutrition enhancers. Wherein the vitamins are indispensable nutrient components in the infant rice flour. The method is particularly important for rapidly and accurately measuring the vitamin content in the infant rice flour at present when the infant rice flour is various in types and has uneven quality. However, when the vitamin content in the infant rice flour is measured by the existing method, the pretreatment operation is complicated, the detection period is long, the reagent consumption is high, and the detection result is inaccurate.
Through the above analysis, the problems and defects of the prior art are as follows: the prior determination method has the disadvantages of complex pretreatment operation, long detection period, high reagent consumption and inaccurate detection result
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a liquid chromatography for measuring the addition of vitamin B12 in infant food and dairy products.
The invention is realized in such a way that the liquid chromatography for measuring the addition amount of vitamin B12 in infant food and dairy products comprises the following steps:
adding a proper amount of sterilized water into infant food and dairy products to be measured, and uniformly stirring to obtain liquid to be measured; filtering and sterilizing the obtained liquid to be measured by utilizing a pre-prepared nanofiber filtering membrane to obtain the liquid to be measured after filtering and sterilizing;
step two, preparing B12 standard working solution: weighing vitamin B12 standard substance, and preparing B12 standard stock solution with concentration not lower than 100 μ g/mL with ultrapure water; diluting the B12 standard stock solution into B12 standard stock solution by using ultrapure water;
step three, establishing a standard working curve: analyzing based on the prepared B12 standard stock solution, and establishing a standard working curve;
step four, detecting the content of vitamin B12 in the solution to be detected by liquid chromatography; and determining the addition amount of the vitamin B12 in the infant food and the dairy product according to the established standard working curve and the detection result of the solution to be detected.
Further, in the first step, the nanofiber filtration membrane preparation method comprises:
(1) adding an additive mixed solution into a pre-prepared nanofiber spinning solution, and uniformly mixing to obtain a nanofiber spinning solution;
(2) coating the obtained nanofiber spinning solution on one or two surfaces of a non-woven fabric supporting layer, and drying at normal temperature to prepare a composite filtering membrane loaded with a nanofiber filtering layer on the surface of the non-woven fabric supporting layer;
(3) soaking the prepared composite filtering membrane in a mixed solution containing a grafting monomer amphoteric compound, and carrying out grafting reaction under certain conditions;
(4) and (3) washing the composite filtering membrane subjected to the grafting reaction, airing at room temperature, sealing and storing to prepare the nanofiber filtering membrane.
Further, the preparation method of the nanofiber spinning solution comprises the following steps:
firstly, taking N, N-dimethylformamide and N, N-dimethylacetamide, and uniformly stirring and mixing to obtain a formamide mixed solution;
secondly, uniformly stirring and mixing the methyl acetamide mixed solution and acetone to obtain a mixed solution, and drying fiber-forming polymer powder to obtain fiber-forming polymer dry powder;
and finally, weighing fiber-forming polymer dry powder, adding the fiber-forming polymer dry powder into the mixed solution, uniformly stirring and mixing, pouring the mixture into a stirring reaction kettle, and stirring to obtain the spinning solution.
Further, the step of drying the fiber-forming polymer powder comprises: and (3) putting the fiber-forming polymer powder into an oven with the temperature of 65-85 ℃ and drying for 22-26 h.
Further, the agitating includes: the temperature is 70-85 ℃, and the stirring speed is 800-1400 r/min.
Further, in step two, the concentration of the B12 standard stock solution was 10. mu.g/mL.
Further, in step three, the establishing of the standard working curve includes:
obtaining a first standard working curve by using a logarithm fitting method for the standard stock solution, obtaining a second standard working curve by using a polynomial fitting method for the standard stock solution, and setting a vitamin B12 concentration conversion value; and generating a vitamin B12-chromatographic intensity curve of the solution to be detected to obtain a standard working curve.
Further, the establishing of the standard working curve further includes:
when the concentration of vitamin B12 in the solution to be detected is less than or equal to the concentration conversion value of vitamin B12, the vitamin B12-chromatographic intensity curve is overlapped with the first standard working curve, and when the concentration of vitamin B12 in the solution to be detected is greater than the concentration conversion value of vitamin B12, the vitamin B12-chromatographic intensity curve is overlapped with the second standard working curve.
Further, in the fourth step, the liquid chromatography conditions are as follows:
a chromatographic column: ACQUITYUPLC BEH C182.1 × 100mm, 1.8 μm;
mobile phase A: 0.1% H3 PO 4, mobile phase B: 80% acetonitrile;
column temperature: 35 ℃; sample introduction amount: 15 mu L of the mixture is prepared into a small volume,
elution time: 0-4 min, 100% A; linearly decreasing to 80% A in 5-15 min; keeping the temperature at 80% A for 16-20 min.
Further, in the fourth step, determining the addition amount of the vitamin B12 in the infant food and the dairy product according to the established standard working curve and the detection result of the solution to be measured includes:
and obtaining a detection result of the solution to be detected, reading the concentration of the vitamin B12 corresponding to the detection spectral intensity of the solution to be detected based on the established standard working curve, and calculating to obtain the content of the vitamin B12 in the sample to be detected.
By combining all the technical schemes, the invention has the advantages and positive effects that: the detection method has high detection accuracy and good repeatability, and can meet the requirements of qualitative and quantitative vitamin detection; the method has the advantages of simple pretreatment, high efficiency, high speed, low consumption, environmental protection, high automation degree, high recovery rate, short detection time and low detection cost. The invention has lower detection limit, wider linear range and good linearity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
FIG. 1 is a flow chart of liquid chromatography for measuring the amount of vitamin B12 added to infant food and milk products according to an embodiment of the present invention.
FIG. 2 is a flow chart of a nanofiber filtration membrane manufacturing method provided in an embodiment of the present invention.
Fig. 3 is a flowchart of a method for preparing a nanofiber spinning solution according to an embodiment of the present invention.
Fig. 4 is a flowchart of a method for establishing a standard operating curve according to an embodiment of the present invention.
Fig. 5 is a flowchart of a method for determining the amount of vitamin B12 added to infant food and milk products according to an established standard working curve and the detection result of the solution to be measured, provided by an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to solve the problems in the prior art, the invention provides a liquid chromatography method for measuring the addition amount of vitamin B12 in infant food and dairy products, and the invention is described in detail with reference to the accompanying drawings.
As shown in fig. 1, the liquid chromatography for determining the addition amount of vitamin B12 in infant food and milk provided in the embodiment of the present invention includes:
s101, adding a proper amount of sterilized water into infant food and dairy products to be measured, and uniformly stirring to obtain liquid to be measured; filtering and sterilizing the obtained liquid to be measured by utilizing a pre-prepared nanofiber filtering membrane to obtain the liquid to be measured after filtering and sterilizing;
s102, preparing a B12 standard working solution: weighing vitamin B12 standard substance, and preparing B12 standard stock solution with concentration not lower than 100 μ g/mL with ultrapure water; diluting the B12 standard stock solution into B12 standard stock solution by using ultrapure water;
s103, establishing a standard working curve: analyzing based on the prepared B12 standard stock solution, and establishing a standard working curve;
s104, detecting the content of vitamin B12 in the solution to be detected by liquid chromatography; and determining the addition amount of the vitamin B12 in the infant food and the dairy product according to the established standard working curve and the detection result of the solution to be detected.
As shown in fig. 2, a method for preparing a nanofiber filtration membrane according to an embodiment of the present invention includes:
s201, adding an additive mixed solution into a pre-prepared nanofiber spinning solution, and uniformly mixing to obtain a nanofiber spinning solution;
s202, coating the obtained nanofiber spinning solution on one or two surfaces of a non-woven fabric supporting layer, and drying at normal temperature to prepare a composite filtering membrane loaded with a nanofiber filtering layer on the surface of the non-woven fabric supporting layer;
s203, soaking the prepared composite filtering membrane in a mixed solution containing a grafting monomer amphoteric compound, and carrying out a grafting reaction under certain conditions;
and S204, washing the composite filtering membrane subjected to the grafting reaction, airing at room temperature, sealing and storing to obtain the nanofiber filtering membrane.
As shown in fig. 3, a method for preparing a nanofiber spinning solution according to an embodiment of the present invention includes:
s301, uniformly stirring and mixing N, N-dimethylformamide and N, N-dimethylacetamide to obtain a formamide mixed solution;
s302, uniformly stirring and mixing the methyl acetamide mixed solution and acetone to obtain a mixed solution, and drying fiber-forming polymer powder to obtain fiber-forming polymer dry powder;
and S303, weighing fiber-forming polymer dry powder, adding the fiber-forming polymer dry powder into the mixed solution, uniformly stirring and mixing, pouring the mixture into a stirring reaction kettle, and stirring to obtain the spinning solution.
The method for drying the fiber-forming polymer powder provided by the embodiment of the invention comprises the following steps: and (3) putting the fiber-forming polymer powder into an oven with the temperature of 65-85 ℃ and drying for 22-26 h.
The stirring provided by the embodiment of the invention comprises the following steps: the temperature is 70-85 ℃, and the stirring speed is 800-1400 r/min.
The concentration of the B12 standard stock solution provided by the embodiment of the invention is 10 mug/mL.
As shown in fig. 4, the establishing of the standard operating curve according to the embodiment of the present invention includes:
s401, obtaining a first standard working curve by using a logarithm fitting method for a standard stock solution;
s402, obtaining a second standard working curve by using a polynomial fitting method for the standard stock solution, and setting a vitamin B12 concentration conversion value;
and S403, generating a vitamin B12-chromatographic intensity curve of the solution to be detected to obtain a standard working curve.
The establishment of the standard working curve provided by the embodiment of the invention further comprises the following steps:
when the concentration of vitamin B12 in the solution to be detected is less than or equal to the concentration conversion value of vitamin B12, the vitamin B12-chromatographic intensity curve is overlapped with the first standard working curve, and when the concentration of vitamin B12 in the solution to be detected is greater than the concentration conversion value of vitamin B12, the vitamin B12-chromatographic intensity curve is overlapped with the second standard working curve.
The liquid chromatographic analysis conditions provided by the embodiment of the invention are as follows:
a chromatographic column: ACQUITYUPLC BEH C182.1 × 100mm, 1.8 μm;
mobile phase A: 0.1% H3 PO 4, mobile phase B: 80% acetonitrile;
column temperature: 35 ℃; sample introduction amount: 15 mu L of the mixture is prepared into a small volume,
elution time: 0-4 min, 100% A; linearly decreasing to 80% A in 5-15 min; keeping the temperature at 80% A for 16-20 min.
As shown in fig. 5, the determination of the added amount of vitamin B12 in infant food and milk products according to the established standard working curve and the detection result of the solution to be tested provided by the embodiment of the present invention includes:
s501, obtaining a detection result of a solution to be detected;
s502, reading the concentration of vitamin B12 corresponding to the detection spectral intensity of the solution to be detected based on the established standard working curve; and calculating to obtain the content of the vitamin B12 in the sample to be detected.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made by those skilled in the art within the technical scope of the present invention disclosed herein, which is within the spirit and principle of the present invention, should be covered by the present invention.

Claims (10)

1. The liquid chromatography for determining the addition of vitamin B12 in infant food and milk products is characterized in that the liquid chromatography for determining the addition of vitamin B12 in infant food and milk products comprises the following steps:
adding a proper amount of sterilized water into infant food and dairy products to be measured, and uniformly stirring to obtain liquid to be measured; filtering and sterilizing the obtained liquid to be measured by utilizing a pre-prepared nanofiber filtering membrane to obtain the liquid to be measured after filtering and sterilizing;
step two, preparing B12 standard working solution: weighing vitamin B12 standard substance, and preparing B12 standard stock solution with concentration not lower than 100 μ g/mL with ultrapure water; diluting the B12 standard stock solution into B12 standard stock solution by using ultrapure water;
step three, establishing a standard working curve: analyzing based on the prepared B12 standard stock solution, and establishing a standard working curve;
step four, detecting the content of vitamin B12 in the solution to be detected by liquid chromatography; and determining the addition amount of the vitamin B12 in the infant food and the dairy product according to the established standard working curve and the detection result of the solution to be detected.
2. The liquid chromatography method for determining the amount of vitamin B12 added to infant food and dairy products according to claim 1, wherein in step one, the nanofiber filtration membrane preparation method comprises:
(1) adding an additive mixed solution into a pre-prepared nanofiber spinning solution, and uniformly mixing to obtain a nanofiber spinning solution;
(2) coating the obtained nanofiber spinning solution on one or two surfaces of a non-woven fabric supporting layer, and drying at normal temperature to prepare a composite filtering membrane loaded with a nanofiber filtering layer on the surface of the non-woven fabric supporting layer;
(3) soaking the prepared composite filtering membrane in a mixed solution containing a grafting monomer amphoteric compound, and carrying out grafting reaction under certain conditions;
(4) and (3) washing the composite filtering membrane subjected to the grafting reaction, airing at room temperature, sealing and storing to prepare the nanofiber filtering membrane.
3. The liquid chromatography method for determining the addition of vitamin B12 in infant food and milk according to claim 2, wherein the preparation method of the nanofiber spinning solution comprises:
firstly, taking N, N-dimethylformamide and N, N-dimethylacetamide, and uniformly stirring and mixing to obtain a formamide mixed solution;
secondly, uniformly stirring and mixing the methyl acetamide mixed solution and acetone to obtain a mixed solution, and drying fiber-forming polymer powder to obtain fiber-forming polymer dry powder;
and finally, weighing fiber-forming polymer dry powder, adding the fiber-forming polymer dry powder into the mixed solution, uniformly stirring and mixing, pouring the mixture into a stirring reaction kettle, and stirring to obtain the spinning solution.
4. The liquid chromatography method of claim 3 for determining the amount of vitamin B12 added to infant food and dairy products wherein said oven drying said powdered fiber-forming polymer comprises: and (3) putting the fiber-forming polymer powder into an oven with the temperature of 65-85 ℃ and drying for 22-26 h.
5. The liquid chromatography method of claim 3 for determining the amount of vitamin B12 added to infant food and dairy products wherein said agitating comprises: the temperature is 70-85 ℃, and the stirring speed is 800-1400 r/min.
6. The liquid chromatography method for determining the amount of vitamin B12 added to infant food and milk according to claim 1, wherein in step two, the concentration of the B12 standard stock solution is 10 μ g/mL.
7. The liquid chromatography method for determining vitamin B12 addition levels in infant food and dairy products of claim 1, wherein in step three, said performing a standard working curve comprises:
obtaining a first standard working curve by using a logarithm fitting method for the standard stock solution, obtaining a second standard working curve by using a polynomial fitting method for the standard stock solution, and setting a vitamin B12 concentration conversion value; and generating a vitamin B12-chromatographic intensity curve of the solution to be detected to obtain a standard working curve.
8. The liquid chromatography method for determining vitamin B12 levels in infant food and dairy products of claim 7, wherein said performing a standard working curve further comprises:
when the concentration of vitamin B12 in the solution to be detected is less than or equal to the concentration conversion value of vitamin B12, the vitamin B12-chromatographic intensity curve is overlapped with the first standard working curve, and when the concentration of vitamin B12 in the solution to be detected is greater than the concentration conversion value of vitamin B12, the vitamin B12-chromatographic intensity curve is overlapped with the second standard working curve.
9. The liquid chromatography method for determining the amount of vitamin B12 added to infant food and dairy products of claim 1, wherein in step four, the liquid chromatography conditions are:
a chromatographic column: ACQUITY UPLC BEH C182.1 × 100mm, 1.8 μm;
mobile phase A: 0.1% H3 PO 4, mobile phase B: 80% acetonitrile;
column temperature: 35 ℃; sample introduction amount: 15 mu L of the mixture is prepared into a small volume,
elution time: 0-4 min, 100% A; linearly decreasing to 80% A in 5-15 min; keeping the temperature at 80% A for 16-20 min.
10. The liquid chromatography method for determining the vitamin B12 addition amount in infant food and dairy products according to claim 1, wherein in step four, the step of determining the vitamin B12 addition amount in infant food and dairy products according to the established standard working curve and the detection result of the solution to be determined comprises the following steps:
and obtaining a detection result of the solution to be detected, reading the concentration of the vitamin B12 corresponding to the detection spectral intensity of the solution to be detected based on the established standard working curve, and calculating to obtain the content of the vitamin B12 in the sample to be detected.
CN202110656055.8A 2021-06-11 2021-06-11 Liquid chromatography for determining vitamin B12 addition in infant food and milk Pending CN113376285A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090111133A1 (en) * 2007-10-31 2009-04-30 Abbott Laboratories Gel Filtration Standard
CN103091442A (en) * 2012-11-13 2013-05-08 江苏艾兰得营养品有限公司 Chromatographic method for determination of vitamin B12 content
WO2013176454A1 (en) * 2012-05-21 2013-11-28 한국콜마주식회사 Method of simultaneous analysis of vitamins using liquid chromatography
CN107271588A (en) * 2017-07-18 2017-10-20 杭州更蓝生物科技有限公司 A kind of method that ultra performance liquid chromatography determines B family vitamin
US20180009838A1 (en) * 2015-01-28 2018-01-11 Charles Sturt University Novel, heavy vitamin b12 derivatives
CN110935325A (en) * 2019-12-31 2020-03-31 杭州帝凡过滤技术有限公司 Ultrahigh-flux nanofiber filtering membrane and preparation method thereof
CN112246113A (en) * 2020-09-07 2021-01-22 武汉纺织大学 Nanofiber filtering membrane with antibacterial and anti-fouling functions and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090111133A1 (en) * 2007-10-31 2009-04-30 Abbott Laboratories Gel Filtration Standard
WO2013176454A1 (en) * 2012-05-21 2013-11-28 한국콜마주식회사 Method of simultaneous analysis of vitamins using liquid chromatography
CN103091442A (en) * 2012-11-13 2013-05-08 江苏艾兰得营养品有限公司 Chromatographic method for determination of vitamin B12 content
US20180009838A1 (en) * 2015-01-28 2018-01-11 Charles Sturt University Novel, heavy vitamin b12 derivatives
CN107271588A (en) * 2017-07-18 2017-10-20 杭州更蓝生物科技有限公司 A kind of method that ultra performance liquid chromatography determines B family vitamin
CN110935325A (en) * 2019-12-31 2020-03-31 杭州帝凡过滤技术有限公司 Ultrahigh-flux nanofiber filtering membrane and preparation method thereof
CN112246113A (en) * 2020-09-07 2021-01-22 武汉纺织大学 Nanofiber filtering membrane with antibacterial and anti-fouling functions and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
ESTHER CAMPOS GIMÉNEZ: "Improved AOAC First Action 2011.08 for the Analysis of Vitamin B12 in Infant Formula and Adult/Pediatric Formulas: First Action 2014.02", 《JOURNAL OF AOAC INTERNATIONAL》 *
何文等: "液相色谱法测定奶粉中维生素B12的研究", 《山东化工》 *
郭建博等: "超高效液相色谱法快速测定复合维生素产品中的10种水溶性维生素", 《食品安全质量检测学报》 *

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