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Simultaneous and rapid determination of nine alcohol compounds in alcohol by gc-ms

A GC-MS, rapid determination technology, applied in the field of analytical chemistry, can solve the problems of large measurement error, low sensitivity, cumbersome operation of colorimetry, etc., and achieve the effect of good precision and low detection limit

Active Publication Date: 2021-08-03
CHINA TOBACCO YUNNAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The operation of colorimetry is cumbersome, low sensitivity, many interference factors, large measurement error, and can only measure a single component
Gas chromatography (FID detector) can also be used to detect the content of alcohol compounds, but due to the low detection sensitivity of the instrument, the test for measuring alcohol often cannot meet the requirements

Method used

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  • Simultaneous and rapid determination of nine alcohol compounds in alcohol by gc-ms
  • Simultaneous and rapid determination of nine alcohol compounds in alcohol by gc-ms
  • Simultaneous and rapid determination of nine alcohol compounds in alcohol by gc-ms

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The method for quickly measuring the content of 9 kinds of alcohol compounds in alcohol by GC-MS simultaneously comprises the following steps:

[0043] Step (1), preparation of internal standard stock solution:

[0044] Use deuterated-1-propanol-1,1,3,3,3-d5 as the internal standard substance and ethanol as the solvent to prepare an internal standard solution with a concentration of 180mg / L as the internal standard stock solution;

[0045] Step (2), sample pretreatment:

[0046] Add ethanol and the internal standard stock solution prepared in step (1) to the alcohol sample to be tested, shake well, let it stand for 1.8 minutes, take the supernatant and filter it through a 0.22 μm organic phase filter membrane, and analyze the filtrate by GC-MS according to Quantification by internal standard method to obtain the ratio of the quantitative ion peak area of ​​9 alcohol compounds in the alcohol sample to be tested to the internal standard deuterated-1-propanol-1,1,3,3,3-d5...

Embodiment 2

[0065] The method for quickly measuring the content of 9 kinds of alcohol compounds in alcohol by GC-MS simultaneously comprises the following steps:

[0066] Step (1), preparation of internal standard stock solution:

[0067] Use deuterated-1-propanol-1,1,3,3,3-d5 as the internal standard substance, and use ethanol as the solvent to prepare an internal standard solution with a concentration of 220 mg / L as the internal standard stock solution;

[0068] Step (2), sample pretreatment:

[0069] Add ethanol and the internal standard stock solution prepared in step (1) to the alcohol sample to be tested, shake well, let it stand for 2.2 minutes, take the supernatant and filter it through a 0.22 μm organic phase filter membrane, and perform GC-MS analysis on the filtrate according to Quantification by internal standard method to obtain the ratio of the quantitative ion peak area of ​​9 alcohol compounds in the alcohol sample to be tested to the internal standard deuterated-1-propan...

Embodiment 3

[0088] The method for quickly measuring the content of 9 kinds of alcohol compounds in alcohol by GC-MS simultaneously comprises the following steps:

[0089] Step (1), preparation of internal standard stock solution:

[0090] Use deuterated-1-propanol-1,1,3,3,3-d5 as the internal standard and ethanol as the solvent to prepare an internal standard solution with a concentration of 200mg / L as the internal standard stock solution;

[0091] Step (2), sample pretreatment:

[0092] Add ethanol and the internal standard stock solution prepared in step (1) to the alcohol sample to be tested, shake well, let it stand still, take the supernatant and filter it through an organic phase filter membrane, analyze the filtrate by GC-MS, and quantify according to the internal standard method , to obtain the ratio of the quantitative ion peak area of ​​the 9 alcohol compounds in the alcohol sample to be tested to the internal standard deuterated-1-propanol-1,1,3,3,3-d5 quantitative ion peak ar...

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Abstract

The invention relates to a method for rapidly determining the contents of nine alcohol compounds in alcohol by using GC-MS, and belongs to the technical field of analytical chemistry. The method includes the steps of preparation of internal standard stock solution, sample pretreatment, drawing of standard working curve, determination of nine kinds of alcohol compounds in the alcohol sample to be tested, and the like. The determination method provided by the invention can be used for 9 kinds of alcohol compounds in alcohol samples, which fills up the gap in the prior art. The method of the present invention is simple, fast and accurate. The nine alcohol compounds have a good linear range within 0.2-10mg / L, the correlation coefficients are all above 0.993, and the quantification limit is between 0.60-0.85 mg / kg. The relative standard deviation of parallel determination results was 1.89%-4.28%, and the recovery rate of standard addition was 88.9%-105.2%. The method has low detection limit, good precision, accuracy and reliability, and has the value of popularization and application.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for rapidly determining the contents of nine alcohol compounds in alcohol by using GC-MS. Background technique [0002] In addition to ethanol and water, a small amount of methanol and fusel oil will be produced during the fermentation process of liquor. Fusel oil is one of the indispensable aroma components in liquor, but the content is too high, and the proportion with acids, esters and other components is out of balance. , which is the main reason for the off-flavor of liquor. At present, there are many analyzes on the content of fusel oil in liquor. Fusel oil is a by-product of alcohol production by fermentation. It is formed during alcohol fermentation and is separated during alcohol distillation. The extraction rate is generally 0.4% to 0.6%. In the process of alcohol extraction and preparation, alcohol compounds will inevitably be produce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 熊文李超范多青王素娟秦云华李娥贤郭丽娟赵敏王璐张子龙
Owner CHINA TOBACCO YUNNAN IND