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Method for analyzing caprylic/capric triglyceride in essence by utilizing gas chromatography-mass spectrometry separation

A caprylic capric acid glyceride and gas chromatography technology, which is applied in the field of gas chromatography-mass spectrometry separation and analysis of caprylic capric acid glyceride in essence, can solve the problem of difficult aroma substances and caprylic capric acid glyceride analysis results, and the influence of flavor components , complex component analysis and other issues, to achieve the effect of improving the peak shape of the chromatographic peak, increasing the resolution, and simplifying the processing method

Inactive Publication Date: 2018-01-12
HUBEI CHINA TOBACCO IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When using GC-MS analysis, because the boiling point of aroma substances is generally relatively low, and the boiling point of caprylic glyceride is relatively high, so if there are such substances in the fragrance or mainly use such substances as solvents, the composition analysis of the fragrance will change. It is more complicated, and it is difficult to take into account the analysis results of aroma substances and caprylic acid glyceride in essence at the same time
Generally, high-performance liquid chromatography or gas chromatography after derivatization pretreatment are often used to analyze such refractory substances. It is not only troublesome, but the most important thing is that the pretreatment process will affect the aroma components in the essence.

Method used

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  • Method for analyzing caprylic/capric triglyceride in essence by utilizing gas chromatography-mass spectrometry separation
  • Method for analyzing caprylic/capric triglyceride in essence by utilizing gas chromatography-mass spectrometry separation
  • Method for analyzing caprylic/capric triglyceride in essence by utilizing gas chromatography-mass spectrometry separation

Examples

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Effect test

Embodiment 1

[0021] Example 1, a method for separating and analyzing caprylic acid glycerides in essence by gas chromatography-mass spectrometry, which specifically analyzes caprylic capric acid glycerides in coffee flavors, and the analysis steps are as follows:

[0022] (1) Sample pretreatment: Take 1g of coffee flavor sample containing caprylic acid glyceride and place it in a conical flask, add 10mL of dichloromethane added with phenylethyl acetate internal standard, and shake it on the shaker at a speed of 90r / min Shake for 20min;

[0023] (2) Oscillation completes, packs into chromatographic vial after filtering with 0.45 micron needle type microporous membrane, sends into gas chromatography-mass spectrometry to analyze, and analysis condition is as follows:

[0024] Chromatographic conditions: chromatographic column is HP-5MS, 30m×0.25μm×0.25mm capillary column; split injection, split ratio is 1:10; carrier gas is high-purity helium, flow rate is 1.0mL / min; injection volume: 1μL ;P...

Embodiment 2

[0031] Embodiment 2, a method for separating and analyzing caprylic-capric glycerides in peppermint essence by gas chromatography-mass spectrometry, which specifically analyzes caprylic-capric glycerides in peppermint essences, and the analysis steps are as follows:

[0032] (1) Sample pretreatment: take 1g of the peppermint flavor sample containing caprylic acid glyceride and place it in a conical flask, add 50mL of dichloromethane added with phenylethyl propionate internal standard, and shake it on the shaker at 120r / min Speed ​​oscillation for 15 minutes;

[0033] (2) Oscillation completes, packs into chromatographic vial after filtering with 0.45 micron needle type microporous membrane, sends into gas chromatography-mass spectrometry to analyze, and analysis condition is as follows:

[0034] Chromatographic conditions: HP-5MS column, 50m×0.25μm×0.25mm capillary column; split injection, split ratio 1:20; carrier gas is high-purity helium, flow rate 1.0mL / min; programmed tem...

Embodiment 3

[0040] Embodiment 3, a method for separating and analyzing caprylic acid glyceride in essence by gas chromatography-mass spectrometry, which specifically analyzes caprylic capric acid glyceride in lemon essence, and the analysis steps are as follows:

[0041] (1) Sample pretreatment: take 0.5g of lemon essence sample and place it in a conical flask, add 10mL of dichloromethane added with phenylethyl acetate as an internal standard, and oscillate on an oscillator at a speed of 100r / min for 20min;

[0042] (2) Oscillation completes, packs into chromatographic vial after filtering with 0.45 micron needle type microporous membrane, sends into gas chromatography-mass spectrometry to analyze, and analysis condition is as follows:

[0043] Chromatographic conditions: chromatographic column is HP-5MS, 30m×0.25μm×0.25mm capillary column; split injection, split ratio is 1:10; carrier gas is high-purity helium, flow rate 1.0mL / min; programmed temperature: initial temperature 80°C; from 2...

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Abstract

The invention provides a method for analyzing caprylic / capric triglyceride in essence by utilizing gas chromatography-mass spectrometry separation. The analyzing method comprises the following steps:adding an organic solvent containing internal standard substances into an essence sample containing caprylic / capric triglyceride, oscillating, filling into a chromatographic bottle, and performing gaschromatography-mass spectrometry analysis under the following conditions: a chromatographic column selecting a low-polar or non-polar column and capillary column having length of 30m, 50m or 60m, a split ratio of 1:10-1:50, carrier gas flow of 0.8-1.5mL / min and sample size of 1-3 mL; and heating to 180 DEG C from the initial temperature of 50-100 DEG C by 2-4 DEG C / min, heating to 250 DEG C by 8-12 DEG C / min, and heating to 325 DEG C by 2-4 DEG C / min, wherein the ion source temperature is 230-280 DEG C, electron energy is 70eV, the scanning range is 100-450, and the solvent delay is 3-10 minutes. The pre-treatment method is simple and easy to operate, has the advantages of low cost, high efficiency and the like, and can be used for increasing the resolution of targeted substances with good repeatability.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis and detection, and in particular relates to a method for separating and analyzing caprylic acid glyceride in essence by using gas chromatography-mass spectrometry. Background technique [0002] Essence is a spice mixture with a certain fragrance type prepared by dissolving several spices in a solvent in a certain proportion and process. Organic solvents for dissolving flavors and fragrances are generally low-carbon chain alcohols such as ethanol, propylene glycol, glycerin, isopropanol, etc., and low-carbon chain or medium-carbon chain esters such as ethyl acetate, caprylic acid glyceride, etc. [0003] Glyceryl Octadecanoate (Glyceryl Octadecanoate, abbreviated as ODO) is made from coconut oil, palm oil, litsea cubeba oil and other oils, through hydrolysis, fractionation, cutting, to obtain caprylic acid, capric acid and glycerol esterification, and then deacidification , dehydration, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 肜霖熊国玺赵国豪马舒翼
Owner HUBEI CHINA TOBACCO IND
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