CN116699039A - Method for rapidly detecting content of phytosterol in DD oil of corn oil removal substance - Google Patents

Method for rapidly detecting content of phytosterol in DD oil of corn oil removal substance Download PDF

Info

Publication number
CN116699039A
CN116699039A CN202310898863.4A CN202310898863A CN116699039A CN 116699039 A CN116699039 A CN 116699039A CN 202310898863 A CN202310898863 A CN 202310898863A CN 116699039 A CN116699039 A CN 116699039A
Authority
CN
China
Prior art keywords
phytosterol
oil
corn oil
content
rapidly detecting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202310898863.4A
Other languages
Chinese (zh)
Inventor
宋立里
崔言峰
王洪章
杨晓飞
李娟�
庄欠虎
李晓龙
吴慧洁
孙钦彩
王一路
庄绪政
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Jinsheng Grain And Oil Food Co ltd
Original Assignee
Shandong Jinsheng Grain And Oil Food Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shandong Jinsheng Grain And Oil Food Co ltd filed Critical Shandong Jinsheng Grain And Oil Food Co ltd
Priority to CN202310898863.4A priority Critical patent/CN116699039A/en
Publication of CN116699039A publication Critical patent/CN116699039A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N11/00—Carrier-bound or immobilised enzymes; Carrier-bound or immobilised microbial cells; Preparation thereof
    • C12N11/02—Enzymes or microbial cells immobilised on or in an organic carrier
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N9/00—Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
    • C12N9/14—Hydrolases (3)
    • C12N9/16—Hydrolases (3) acting on ester bonds (3.1)
    • C12N9/18—Carboxylic ester hydrolases (3.1.1)
    • C12N9/20—Triglyceride splitting, e.g. by means of lipase
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12Y—ENZYMES
    • C12Y301/00—Hydrolases acting on ester bonds (3.1)
    • C12Y301/01—Carboxylic ester hydrolases (3.1.1)
    • C12Y301/01003—Triacylglycerol lipase (3.1.1.3)
    • 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
    • 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
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • 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
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography
    • 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
    • G01N2030/067—Preparation by reaction, e.g. derivatising the sample
    • 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
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Biochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Zoology (AREA)
  • Wood Science & Technology (AREA)
  • Genetics & Genomics (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Immunology (AREA)
  • General Engineering & Computer Science (AREA)
  • General Physics & Mathematics (AREA)
  • Biomedical Technology (AREA)
  • Biotechnology (AREA)
  • Microbiology (AREA)
  • Medicinal Chemistry (AREA)
  • Molecular Biology (AREA)
  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)

Abstract

The invention relates to the technical field of vegetable oil detection, and discloses a method for rapidly detecting the content of phytosterol in corn oil removal DD oil. Mixing corn oil removed DD oil and methanol, shaking, adding immobilized lipase, reacting to obtain phytosterol, melting diethyl ether, diluting with n-hexane, and calculating the content of cholestanol by gas chromatography and peak area.

Description

Method for rapidly detecting content of phytosterol in DD oil of corn oil removal substance
Technical Field
The invention relates to the technical field of vegetable oil detection, in particular to a method for rapidly detecting the content of phytosterol in corn oil remover DD oil.
Background
Enzymes are produced by living cells, highly specific and highly catalytic proteins or RNAs, a class of biocatalysts. The enzyme has the characteristics of high efficiency, specificity, mildness, adjustability and the like, and is widely applied to the fields of brewing wine, wheaten food, medical treatment and the like. The enzyme is embedded in the water insoluble macromolecule by a physical or chemical method, so that the enzyme can be repeatedly used for many times. Several methods are currently in common use, adsorption, cross-linking, covalent bonding and entrapment. For example, the development of a novel immobilization technology is reported in the text of preparation and application of immobilized enzyme, ultrasonic waves are utilized to lead a polymer main chain to be homolytic, thereby triggering functional monomers to synthesize a block copolymer carrier, and a general polymer is modified into a novel enzyme immobilization carrier by means of a modern technology.
The phytosterol is a functional component combined by fatty acid and sugar, has strong anti-inflammatory property, has obvious curative effects on certain heart diseases, ulcers, cancers and the like, and is widely applied to industries such as foods, health-care products, medicines and the like. Natural vegetable oil deodorized distillate contains a large amount of plant sterols, and digitonin is often used in the early stage, and is rarely used in recent years due to high cost. The conventional measurement methods are thin layer chromatography, visible light colorimetric method, gas chromatography and high performance liquid chromatography, which are all faster, lower in cost and simpler and more convenient to operate. Gas chromatography is also currently the most commonly used test method, pretreatment before detection: 0.1 g of cholesterol as an internal standard is weighed to be 0.001g, ethanol potassium hydroxide is added, the mixture is subjected to shaking table treatment for 60 minutes in a water bath at 60 ℃, n-hexane is extracted twice, nitrogen blowing is carried out, 200 mu l of BSTFA+TMCS is added for reaction at 105 ℃ for 15 minutes, and the mixture is subjected to on-machine detection through a 0.22 mu m filter head.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides the method for rapidly detecting the content of the phytosterol in the DD oil of the corn oil removal product, which improves the performance and the crosslinking degree of the crosslinking agent, improves the immobilization rate of lipase, greatly increases the extraction rate of the phytosterol, simultaneously ensures the repeated use of the immobilized enzyme, and further ensures the accuracy of the detection result.
(II) technical scheme
(1) Dissolving gelatin in distilled water at 38-45 deg.c, stirring to dissolve for 10-30min, adding styrene, divinylbenzene and trimethylol propane trimethyl acrylate successively at 75-80 deg.c, stirring to react for 1-3 hr, heating to react, and vacuum drying to obtain polymer microsphere.
(2) Adding lipase and microspheres into the phosphate buffer solution, standing for reaction for 24-48h, adding the phosphate buffer solution into the solution at 20-35 ℃, magnetically stirring the solution for 8-10h, standing, washing with distilled water, washing with the phosphate buffer solution, filtering and drying to obtain the immobilized lipase.
(3) Adding corn oil removal DD oil and methanol into a flask, shaking uniformly, adding immobilized lipase into the flask, performing shaking reaction through a shaking table, cooling, crystallizing, and filtering to obtain the phytosterol.
(4) Dissolving the obtained phytosterol in diethyl ether, adding n-hexane, passing through a micro-filtration pore membrane of 0.15-0.25 μm, and measuring on a machine; and (3) analyzing by using a gas chromatography, and calculating to obtain the content of the phytosterol according to the peak area by using the cholestanol as an internal standard substance.
Preferably, the mass ratio of the styrene to the divinylbenzene to the trimethylolpropane trimethacrylate in the step (1) is 1:0.9-1.3:0.08-0.15.
Preferably, the step (1) of heating reaction comprises the following steps: heating to 85-95 ℃, reacting for 1-3h, heating to 95-98 ℃ and reacting for 1-3h.
Preferably, the molar concentration of the phosphate buffer solution in the step (2) is 0.03-0.06mol/mL.
Preferably, the shaking table in the step (3) is oscillated for 10-30 hours.
Preferably, the type of the chromatographic column in the step (4) is 19091J-413, and the flow rate is 1-1.4mL/min; the temperature of the sample inlet is 260-300 ℃, the carrier gas is helium, the split sample is introduced, and the split ratio is 15-30:1, column temperature 250-270 ℃, detector 280-300 ℃.
(III) beneficial technical effects
Dissolving gelatin, and then mixing and dissolving with styrene, divinylbenzene and trimethylolpropane trimethacrylate to obtain polymer microspheres; mixing lipase and microspheres in a phosphate buffer solution for reaction to obtain immobilized lipase; mixing corn oil removed DD oil and methanol uniformly, adding immobilized lipase for reaction to obtain phytosterol; after the diethyl ether is melted, the mixture is diluted by normal hexane, the cholestanol is used as an internal standard substance, and the gas chromatographic analysis and the peak area calculation are carried out. The lipase enzyme is immobilized by a crosslinking method, the immobilization rate of the lipase in unit area is high, and simultaneously, the trimethylolpropane trimethacrylate is added, so that the crosslinking degree of the lipase and the polymer microsphere can be greatly improved, and the immobilization rate of the lipase is improved. The phytosterol in the corn oil removal DD oil is extracted by an enzyme method, the enzyme method is efficient and clean, pollution is avoided, the immobilized enzyme can be reused, and resources are saved. The enzyme method has the advantages of higher extraction efficiency, high extraction rate of the phytosterol, no generation of additional substances, no generation of too much error in subsequent detection, mild condition, simple operation and guaranteed accuracy. The invention adopts a gas chromatograph, which is the main stream detection method at present, the analysis of the types and the content of sterols is more comprehensive, and the subsequent data result is more visual.
Drawings
FIG. 1 is a graph showing the effect of the amount of enzyme added on the esterification rate.
FIG. 2 is a graph showing the effect of the amount of methanol added on the esterification rate.
FIG. 3 is a test of the effect of reaction time on the esterification rate.
Detailed Description
Example 1: (1) Dissolving gelatin in distilled water at 40 ℃, stirring and dissolving for 15min, sequentially adding 15g of styrene, 20g of divinylbenzene and 1.2g of trimethylolpropane trimethacrylate into the mixture at 78 ℃, stirring and reacting for 2h, and then heating and reacting: heating to 90 ℃, reacting for 2 hours, heating to 96 ℃, reacting for 2 hours, and vacuum drying to obtain the polymer microsphere.
(2) Adding lipase and microspheres into 0.03mol/mL phosphate buffer solution, standing for reaction for 24 hours, adding the phosphate buffer solution into the solution at 20 ℃, magnetically stirring the solution for 8 hours, standing, washing with distilled water, washing with the phosphate buffer solution, filtering and drying to obtain the immobilized lipase.
(3) Adding corn oil removal DD oil and methanol into a flask, shaking uniformly, adding immobilized lipase into the flask, carrying out shaking reaction for 10 hours by a shaking table, cooling, crystallizing, and filtering to obtain the phytosterol.
(4) Dissolving the obtained phytosterol in diethyl ether, adding n-hexane, passing through a 0.15 μm microfiltration pore membrane, and measuring on a machine; analyzing by gas chromatography, wherein the model of the chromatographic column is 19091J-413, and the flow rate is 1mL/min; the temperature of the sample inlet is 260 ℃, the carrier gas is helium, the split sample is introduced, and the split ratio is 15:1, column temperature 250 ℃, detector 280 ℃, cholestanol as an internal standard, and calculating according to peak area to obtain the content of the phytosterol.
Example 2: (1) Dissolving gelatin in distilled water at 42 ℃, stirring and dissolving for 20min, sequentially adding 13g of styrene, 16g of divinylbenzene and 1.2g of trimethylolpropane trimethacrylate into the mixture at 80 ℃, stirring and reacting for 3h, and then heating and reacting: heating to 92 ℃ for reaction for 1h, heating to 95 ℃ for reaction for 2h, and vacuum drying to obtain the polymer microsphere.
(2) Adding lipase and microspheres into 0.04mol/mL phosphate buffer solution, standing for reaction for 30h, adding the phosphate buffer solution into the solution at 30 ℃, magnetically stirring the solution for 9h, standing, washing with distilled water, washing with the phosphate buffer solution, filtering and drying to obtain the immobilized lipase.
(3) Adding corn oil removal DD oil and methanol into a flask, shaking uniformly, adding immobilized lipase into the flask, carrying out shaking reaction for 30 hours by a shaking table, cooling, crystallizing, and filtering to obtain the phytosterol.
(4) Dissolving the obtained phytosterol in diethyl ether, adding n-hexane, passing through a 0.22 μm microfiltration pore membrane, and measuring on a machine; analyzing by gas chromatography, wherein the model of the chromatographic column is 19091J-413, and the flow rate is 1.2mL/min; the temperature of the sample inlet is 280 ℃, the carrier gas is helium, the split sample is introduced, and the split ratio is 20:1, column temperature 260 ℃, detector 280 ℃, cholestanol is used as an internal standard substance, and the content of the phytosterol is calculated according to peak area.
Example 3: (1) Dissolving gelatin in distilled water at 38 ℃, stirring and dissolving for 10min, sequentially adding 5g of styrene, 10g of divinylbenzene and 0.5g of trimethylolpropane trimethacrylate into the mixture at 75 ℃, stirring and reacting for 1h, and then heating and reacting: heating to 85 ℃, reacting for 1h, heating to 95 ℃, reacting for 1h, and vacuum drying to obtain the polymer microsphere.
(2) Adding lipase and microspheres into 0.06mol/mL phosphate buffer solution, standing for reaction for 48h, adding the phosphate buffer solution into the solution at 35 ℃, magnetically stirring the solution for 10h, standing, washing with distilled water, washing with the phosphate buffer solution, filtering and drying to obtain the immobilized lipase.
(3) Adding corn oil removal DD oil and methanol into a flask, shaking uniformly, adding immobilized lipase into the flask, carrying out shaking reaction for 15h through a shaking table, cooling, crystallizing, and filtering to obtain the phytosterol.
(4) Dissolving the obtained phytosterol in diethyl ether, adding n-hexane, passing through a micro-filtration pore membrane of-0.25 μm, and measuring by a machine; analyzing by gas chromatography, wherein the model of the chromatographic column is 19091J-413, and the flow rate is 1.4mL/min; the temperature of the sample inlet is 300 ℃, the carrier gas is helium, the split sample is introduced, and the split ratio is 30:1, column temperature 270 ℃, detector 300 ℃, cholestanol is used as an internal standard substance, and the content of the phytosterol is calculated according to peak area.
Example 4: (1) Dissolving gelatin in distilled water at 45 ℃, stirring and dissolving for 30min, sequentially adding 10g of styrene, 12g of divinylbenzene and 1g of trimethylolpropane trimethacrylate into the mixture at 80 ℃, stirring and reacting for 3h, and then heating and reacting: heating to 95 ℃ for reaction for 3 hours, heating to 98 ℃ for reaction for 3 hours, and vacuum drying to obtain the polymer microsphere.
(2) Adding lipase and microspheres into 0.05mol/mL phosphate buffer solution, standing for reaction for 40h, adding the phosphate buffer solution into the solution at 25 ℃, magnetically stirring the solution for 10h, standing, washing with distilled water, washing with the phosphate buffer solution, filtering and drying to obtain the immobilized lipase.
(3) Adding corn oil removal DD oil and methanol into a flask, shaking uniformly, adding immobilized lipase into the flask, carrying out shaking reaction for 18h through a shaking table, cooling, crystallizing, and filtering to obtain the phytosterol.
(4) Dissolving the obtained phytosterol in diethyl ether, adding n-hexane, passing through a 0.18 μm microfiltration pore membrane, and measuring on a machine; analyzing by gas chromatography, wherein the model of the chromatographic column is 19091J-413, and the flow rate is 1mL/min; the temperature of the sample inlet is 300 ℃, the carrier gas is helium, the split sample is introduced, and the split ratio is 30:1, column temperature 255 ℃, detector 285 ℃, cholestanol as an internal standard, and calculating according to peak area to obtain the content of the phytosterol.
Example 5: (1) Dissolving gelatin in distilled water at 40 ℃, stirring and dissolving for 25min, sequentially adding 11g of styrene, 10g of divinylbenzene and 0.8g of trimethylolpropane trimethacrylate into the mixture at 80 ℃, stirring and reacting for 1h, and then heating and reacting: heating to 85 ℃, reacting for 3 hours, heating to 95 ℃, reacting for 2 hours, and vacuum drying to obtain the polymer microsphere.
(2) Adding lipase and microspheres into 0.06mol/mL phosphate buffer solution, standing for reaction for 24 hours, adding the phosphate buffer solution into the solution at 20-35 ℃, magnetically stirring the solution for 9 hours, standing, washing with distilled water, washing with the phosphate buffer solution, filtering and drying to obtain the immobilized lipase.
(3) Adding corn oil removal DD oil and methanol into a flask, shaking uniformly, adding immobilized lipase into the flask, carrying out shaking reaction for 30 hours by a shaking table, cooling, crystallizing, and filtering to obtain the phytosterol.
(4) Dissolving the obtained phytosterol in diethyl ether, adding n-hexane, passing through a 0.15 μm microfiltration pore membrane, and measuring on a machine; analyzing by gas chromatography, wherein the model of the chromatographic column is 19091J-413, and the flow rate is 1.3mL/min; the temperature of the sample inlet is 270 ℃, the carrier gas is helium, the split sample is introduced, and the split ratio is 20:1, column temperature 270 ℃, detector 280 ℃, cholestanol is used as an internal standard substance, and the content of the phytosterol is calculated according to peak area.
TABLE 1 content of major phytosterols in corn oil removal DD oil
The invention adopts a gas chromatograph, which is the main stream detection method at present, the analysis of the types and the content of sterols is more comprehensive, and the subsequent data result is more visual.

Claims (6)

1. A method for rapidly detecting the content of phytosterol in corn oil remover DD oil is characterized by comprising the following steps: the detection method comprises the following steps:
(1) Dissolving gelatin in distilled water at 38-45 ℃, stirring and dissolving for 10-30min, sequentially adding styrene, divinylbenzene and trimethylolpropane trimethacrylate into the mixture at 75-80 ℃, stirring and reacting for 1-3h, heating and reacting, and vacuum drying to obtain polymer microspheres;
(2) Adding lipase and microspheres into a phosphate buffer solution, standing for reaction for 24-48h, adding the phosphate buffer solution into the solution at 20-35 ℃, magnetically stirring the solution for 8-10h, standing, washing with distilled water, washing with the phosphate buffer solution, filtering and drying to obtain immobilized lipase;
(3) Adding corn oil removal DD oil and methanol into a flask, shaking uniformly, adding immobilized lipase into the flask, carrying out shaking reaction by a shaking table, cooling, crystallizing and filtering to obtain phytosterol;
(4) Dissolving the obtained phytosterol in diethyl ether, adding n-hexane, passing through a micro-filtration pore membrane of 0.15-0.25 μm, and measuring on a machine; and (3) analyzing by using a gas chromatography, and calculating to obtain the content of the phytosterol according to the peak area by using the cholestanol as an internal standard substance.
2. The method for rapidly detecting the phytosterol content in the corn oil remover DD oil according to claim 1, which is characterized by comprising the following steps: in the step (1), the mass ratio of the styrene to the divinylbenzene to the trimethylolpropane trimethacrylate is 1:0.9-1.3:0.08-0.15.
3. The method for rapidly detecting the phytosterol content in the corn oil remover DD oil according to claim 1, which is characterized by comprising the following steps: the temperature rising reaction step in the step (1) is as follows: heating to 85-95 ℃, reacting for 1-3h, heating to 95-98 ℃ and reacting for 1-3h.
4. The method for rapidly detecting the phytosterol content in the corn oil remover DD oil according to claim 1, which is characterized by comprising the following steps: the molar concentration of the phosphoric acid buffer solution in the step (2) is 0.03-0.06mol/mL.
5. The method for rapidly detecting the phytosterol content in the corn oil remover DD oil according to claim 1, which is characterized by comprising the following steps: and (3) the shaking table shake reaction time in the step (3) is 10-30 hours.
6. The method for rapidly detecting the phytosterol content in the corn oil remover DD oil according to claim 1, which is characterized by comprising the following steps: the model of the chromatographic column in the step (4) is 19091J-413, and the flow speed is 1-1.4mL/min; the temperature of the sample inlet is 260-300 ℃, the carrier gas is helium, the split sample is introduced, and the split ratio is 15-30:1, column temperature 250-270 ℃, detector 280-300 ℃.
CN202310898863.4A 2023-07-21 2023-07-21 Method for rapidly detecting content of phytosterol in DD oil of corn oil removal substance Pending CN116699039A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310898863.4A CN116699039A (en) 2023-07-21 2023-07-21 Method for rapidly detecting content of phytosterol in DD oil of corn oil removal substance

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310898863.4A CN116699039A (en) 2023-07-21 2023-07-21 Method for rapidly detecting content of phytosterol in DD oil of corn oil removal substance

Publications (1)

Publication Number Publication Date
CN116699039A true CN116699039A (en) 2023-09-05

Family

ID=87831304

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310898863.4A Pending CN116699039A (en) 2023-07-21 2023-07-21 Method for rapidly detecting content of phytosterol in DD oil of corn oil removal substance

Country Status (1)

Country Link
CN (1) CN116699039A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030100044A1 (en) * 2001-08-22 2003-05-29 Diaz Miguel Angel Fuenzalida Selective transesterification of stanols in mixtures comprising sterols and stanols
DE60215729D1 (en) * 2001-08-22 2006-12-14 Haerting Thomas Francis Selective transesterification of stanols in mixtures containing sterols and stanols
CN103045664A (en) * 2012-12-15 2013-04-17 华中科技大学 Method for producing biodiesel, sterol and vitamin E from deodorized distillate
CN113249369A (en) * 2021-03-26 2021-08-13 河北工业大学 Immobilized lipase and preparation method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030100044A1 (en) * 2001-08-22 2003-05-29 Diaz Miguel Angel Fuenzalida Selective transesterification of stanols in mixtures comprising sterols and stanols
DE60215729D1 (en) * 2001-08-22 2006-12-14 Haerting Thomas Francis Selective transesterification of stanols in mixtures containing sterols and stanols
CN103045664A (en) * 2012-12-15 2013-04-17 华中科技大学 Method for producing biodiesel, sterol and vitamin E from deodorized distillate
CN113249369A (en) * 2021-03-26 2021-08-13 河北工业大学 Immobilized lipase and preparation method and application thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
国家食品药品监督管理局职业药师资格认证中心编写: "《国家职业药师自考考试应试指南 药学专业知识（二）》", 中国中医药出版社, pages: 244 *
房涛 等: "玉米油中植物甾醇的检测方法研究", 《粮食与食品工业》, vol. 22, no. 2, pages 90 - 93 *
淳宏 等: "固定化脂肪酶催化酯交换合成生物柴油研究", 《粮食与油脂》, no. 8, pages 12 - 15 *
肖勇生等: "脱臭馏出物中酶法合成脂肪酸甲酯及提取植物甾醇的研究", 《安徽农业科学》, vol. 41, no. 21, pages 9051 - 9052 *

Similar Documents

Publication Publication Date Title
CN100446844C (en) Nylon affinity membrane preparing method and use
CN113295806B (en) Method for detecting 9 cholesterol oxides in food by gas chromatography-mass spectrometry
CN111650286A (en) Method for detecting medium-long chain fatty acid in human serum based on gas chromatography-mass spectrometry
CN104569399A (en) Test strip for testing ochratoxin A and application of test strip
CN106645509A (en) Detection method for antibiotic residue in milk
Li et al. Preparation and properties of rhizopus oryzae lipase immobilized using an adsorption-crosslinking method
CN116699039A (en) Method for rapidly detecting content of phytosterol in DD oil of corn oil removal substance
CN101380551B (en) Preparation method of nylon affinity membrane and use thereof
CN105319366A (en) Time-resolved fluorescence immunoassay kit detecting methyl parathion and detection method thereof
CN106381268A (en) Method for continuously hydrolyzing cellobiose in straws by using immobilized enzyme microreactor
US20240115971A1 (en) Method for Extracting and Separating Various Components from Flaxseed Meal based on Subcritical Composite Solvent
CN103792347A (en) Special test box for enzyme-linked immunosorbent assay of class-B trichothecenes
CN1696698A (en) Affinity chromatography-enzyme immunoassay method for PAT protein, and dedicated kit
CN102590210B (en) Method for measuring content of alpha-glucosin cane juice
CN109536477A (en) A kind of method of immobilized β-glucosidase production gentian oligose
CN106124716B (en) A kind of Clenbuterol rapid detection method
CN109507247A (en) Identify the method in the millet place of production based on nonlinear chemical fingerprint
CN114875015A (en) Preparation method of lipase-polymer conjugate and application of lipase-polymer conjugate in structural lipid transesterification
Meyer et al. Immobilization of enzymes in liquid membranes for enantioselective hydrolysis
CN104792896A (en) Heparanase composition capable of complete specific enzymolysis of enoxaparin sodium and application of heparanase composition
JPS6121098A (en) Preparation of enzymic reaction product
CN104419689B (en) The bio-affinity purifying method of hyaluronidase
CN112924578B (en) Detection method for simultaneously determining hemicellulose and cellulose in peach fruits
CN114717056B (en) Method for acid-catalyzed methyl esterification of grease
CN113880779B (en) Extraction method of phenamine mycin

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination