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A pretreatment method for measuring a stable oxygen isotope ratio in glycerol in edible oil

An oxygen isotope and edible oil technology, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of easy explosion of lithium aluminum hydride and cumbersome pretreatment process.

Inactive Publication Date: 2016-04-20
CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that the pretreatment process of this method is extremely cumbersome, and lithium aluminum hydride is a dangerous product (explosive when exposed to water), and there are certain safety risks in the process of use and storage

Method used

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  • A pretreatment method for measuring a stable oxygen isotope ratio in glycerol in edible oil
  • A pretreatment method for measuring a stable oxygen isotope ratio in glycerol in edible oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1 Material method

[0023] 1.1 Instrument

[0024] Gas chromatograph (TraceGC), cracking conversion device (ISOLink), stable isotope ratio mass spectrometer (DeltaVAdvantage), the above instruments were purchased from Thermo Fisher Scientific (China) Co., Ltd.;

[0025] Constant temperature water bath (Beijing Shentai Weiye Instrument Equipment Co., Ltd.). Electronic Analytical Balance (Mettler-Toledo International AG).

[0026] 1.2 Reagents

[0027] Vegetable oil; Supersaturated methanolic potassium hydroxide solution; Concentrated hydrochloric acid.

[0028] 1.3 Chromatographic conditions

[0029] CP-Wax capillary column (25m*0.25mm*0.20μm); the carrier gas is helium; the column flow rate is 1.2mL / min; the inlet temperature is 270°C; Raise the temperature at 20°C / min to 220°C and keep for 7min; the injection volume is 1μL; the split ratio is 20:1.

[0030] 1.4 Working conditions of cracking unit

[0031] The pyrolysis tube (ceramic tube with platinum tube insid...

Embodiment 2

[0043] Using the sample pretreatment method and measurement conditions in Example 1, select a corn oil as the research object, get 5 parts of oil after processing and measure the glycerol δ 18 O, the results are shown in Table 2.

[0044] Table 2 Glycerol δ of corn oil 18 ORepeated determination results

[0045] sample

[0046] It can be seen from Table 2 that the continuous determination of glycerol δ in corn oil 18 The standard deviation of O is 0.47‰.

Embodiment 3

[0048] Verify that the present invention measures glycerol δ 18 The accuracy of O, in corn oil, mixes 10%, 25%, 50%, 75% glycerol (glycerin reagent) by glycerol content, uses the sample pretreatment method and the measuring condition in the embodiment one after mixing homogeneously Determination of glycerol δ of each simulated sample 18 O value, the results are shown in the appendix figure 2 .

[0049] attached figure 2 In the simulated sample, glycerol δ 18 The measured value of O changes with the incorporation of glycerol, and has a linear positive correlation with the incorporation of glycerol (R 2 =0.95), which shows that the pretreatment step and analysis method involved in this invention can accurately measure the glycerol δ of edible oil 18 O value.

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Abstract

The invention relates to a pretreatment method for measuring a stable oxygen isotope ratio in glycerol in edible oil. The method includes firstly converting triglyceride in the edible oil into free glycerol through transesterification, and removing fatty acid methyl esters and free fatty acids through an extraction technique. By the pretreatment method, stable oxygen isotope composition of the glycerol can be measured with a gas chromatography-pyrolysis-stable isotope ratio mass spectrometer. The method is safe, efficient, simple in operation and suitable for measuring the stable oxygen isotope ratio in the glycerol in the edible oil.

Description

Technical field: [0001] The present invention relates to the stable oxygen isotope ratio (denoted as δ 18 O) pretreatment method. Specifically, the glycerol in the edible oil is freed from the sample through transesterification, the fatty acid methyl ester is removed by liquid-liquid extraction, and the δ 18 O, belongs to the technical field of stable isotope analysis. Background technique: [0002] Edible oil is an indispensable food in people's daily life, but there are large differences in nutritional value and market price of edible oil due to different types and sources. my country is the largest producer and consumer of edible oil in the world. The consumption of edible oil is increasing year by year. With the improvement of living standards, vegetable oil rich in unsaturated fatty acids, especially high-grade vegetable oil, is more and more favored by consumers. However, due to the imperfect access system of my country's edible oil industry and low production stand...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025G01N2030/065
Inventor 钟其顶王道兵
Owner CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD