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Gas chromatography method for detecting C18 fatty acid in grease

A gas chromatography and fatty acid technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to separate C18 fatty acid isomers, difficult separation, low detection limit of separation efficiency, etc., to achieve easy popularization and application, method Stable, easy-to-use effects

Active Publication Date: 2017-02-22
INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the close physical and chemical properties of C18 fatty acid isomers, it is difficult to completely separate the isomers by conventional fatty acid analysis methods
[0004] Gas chromatography is widely used in the detection of fatty acid isomers in vegetable oils due to its high separation efficiency and low detection limit. No gas chromatographic column can completely separate C18 fatty acid isomers

Method used

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  • Gas chromatography method for detecting C18 fatty acid in grease
  • Gas chromatography method for detecting C18 fatty acid in grease
  • Gas chromatography method for detecting C18 fatty acid in grease

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] Embodiment 1 adopts the method of the present invention to carry out gas chromatography analysis of C18 fatty acid isomers to vegetable oil.

[0083] Pretreatment: Qualitative and quantitative analysis of C18 isomers in oils:

[0084] Weigh 200mg of linseed oil, perilla oil, soybean oil and corn oil into 10mL centrifuge tubes respectively, add 2mL of C11:0 internal standard solution, then add 0.1mL of 2mol / L potassium hydroxide methanol solution, and vortex to mix Uniform 30s. Centrifuge at 4000 rpm for 10 min. Take 20 μL of the supernatant and dilute it to a 1 mL volumetric flask, and use Shimadzu GC-2010 gas chromatography for measurement. The chromatographic column is SLB-IL111 (200m×0.25mm×0.20μm).

[0085] Chromatographic conditions, inlet temperature: 230°C; injection volume: 1 μL; split ratio: 60:1.

[0086] The initial temperature of the chromatographic column is 60°C. After keeping for 5 minutes, the temperature is raised to 175°C at 10°C / min, and then kept ...

Embodiment 2

[0093] Example 2 The gas chromatography analysis of C18 fatty acid isomers is carried out on animal oil by adopting the method of the present invention.

[0094] Pretreatment: Qualitative and quantitative analysis of C18 isomers in oils:

[0095] Weigh 200mg of animal oil into 10mL centrifuge tubes, add 2mL of C11:0 internal standard solution, then add 0.1mL of 3.5mol / L potassium hydroxide methanol solution, and vortex for 30s. Centrifuge at 4000 rpm for 10 min. Take 20 μL of the supernatant and dilute it to a 1 mL volumetric flask, and use Shimadzu GC-2010 gas chromatography for measurement. The chromatographic column is SLB-IL111 (200m×0.25mm×0.20μm).

[0096] Chromatographic conditions, inlet temperature: 200°C; injection volume: 1 μL; split ratio: 80:1.

[0097] The initial temperature of the chromatographic column is 70°C. After keeping for 5 minutes, the temperature is raised to 175°C at 15°C / min, and then kept for 22 minutes, then raised to 185°C at 3°C / min, and kept ...

Embodiment 3

[0103] Example 3 Gas chromatography analysis of C18 fatty acid isomers was carried out on animal milk by using the method of the present invention.

[0104] Pretreatment: Qualitative and quantitative analysis of C18 isomers in animal milk:

[0105] Weigh 200mg of milk and place them in 10mL centrifuge tubes, add 2mL of C11:0 internal standard solution and 3mL of toluene, then add 4mL of 10% acetyl chloride methanol solution, fill with nitrogen for 1min, vortex mix in 80℃ water bath for 2h, every 20min Shake once, take out and cool to room temperature, transfer to 30mL centrifuge tube, wash 3 times with 3mL 6% sodium carbonate solution, combine into 30mL centrifuge tube, mix well, centrifuge at 5000r / min for 5min, take supernatant, use It was determined by Shimadzu GC-2010 gas chromatography, and the chromatographic column was SLB-IL111 (200m×0.25mm×0.20μm).

[0106] Chromatographic conditions, inlet temperature: 230°C; injection volume: 1 μL; split ratio: 100:1.

[0107] The...

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Abstract

The invention discloses a gas chromatography method for detecting C18 fatty acid isomers in grease. A high-polarity ionic liquid gas chromatographic column with the specifications of 200 m*0.25 mm*0.20 mu m is used for detecting the C18 fatty acid isomers in the grease. By means of the method, the separation degree of C18:1 and C18:2 isomers is improved and C18:3 isomers are effectively separated. According to the established C18 fatty acid isomer method, the RSD (relative standard deviation) of the within-day precision is controlled in the range of 0.83%-4.30%, the RSD of the day to day precision is controlled in the range of 1.53%-3.90%, and the quantitative analysis requirements are met. According to the established C18 fatty acid isomer method, the detection limit ranges from 0.009 mg / L to 0.075 mg / L, and the minimum determination limit ranges from 0.028 mg / L to 0.225 mg / L, and the detection limit and the determination limit of C18 cis-trans-isomers are remarkably reduced.

Description

technical field [0001] The invention relates to the technical field of oil detection, in particular to a gas chromatography method for detecting C18 fatty acids in oil. Background technique [0002] In daily life, oily foods are consumed every day, but the vegetable oil, animal oil or animal milk used to process these foods, such as soybean oil, rapeseed oil, sunflower oil, lard or milk, will produce trans fatty acids during high temperature processes, especially Many unscrupulous vendors use frying oil in the waste oil category for cooking and processing food. The large amount of trans fatty acids contained in these low-quality oils cause serious harm to the nutrition and health of consumers, and the trans fatty acids in high-temperature vegetable oil are different The conformers are mainly derived from C18 unsaturated fatty acids. [0003] The C18 unsaturated fatty acids in vegetable oils are oleic acid, linoleic acid and linolenic acid, which will undergo isomerization r...

Claims

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Application Information

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IPC IPC(8): G01N30/68G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N30/68
Inventor 哈益明姜帆郭芹李庆鹏靳婧
Owner INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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