Preparation method of special capillary chromatographic column for detecting Baijiu

A capillary chromatographic column and capillary column technology, which is applied in the field of preparation of special capillary chromatographic columns for liquor detection, can solve the problems of affecting the service life of PEG-20M capillary columns, affecting accurate quantification, tailing of acid substances, etc., and achieve long service life , improve quantitative accuracy, and low cost

Active Publication Date: 2018-04-24
兰州东立龙信息技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the large-aperture liquor LZP-930 chromatographic column in GB / T10345 and CN00123364 has solved the separation problem of methanol and ethyl acetate in liquor, it can only do more than 20 kinds of aroma components in liquor, and in this type of fixed The peak shape and tail of the acid substances in the liquor in the liquid affect the accurate quantification
Although PEG-20M capillary chromatographic columns can meet the requirements of direct sample analysis of alcohols, esters, aldehydes, and ketones in liquor, and can also directly determine the content of organic acids and even high-carbon fatty acid ethyl esters, such polar capillary chromatographic columns Ethyl acetate and acetal cannot be separated, so it needs to be determined by packed column chromatography, and the large amount of water contained in low-alcohol liquor will also affect the service life of PEG-20M capillary column

Method used

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  • Preparation method of special capillary chromatographic column for detecting Baijiu
  • Preparation method of special capillary chromatographic column for detecting Baijiu

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 The preparation method of a special capillary chromatographic column for liquor detection comprises the following steps:

[0024] (1) First rinse the inner wall of the elastic quartz capillary column with 1 mol / L HCl, then rinse the inner wall of the elastic quartz capillary column with water for 3 times, and finally install the rinsed elastic quartz capillary column on the chromatographic instrument, and purge it with nitrogen. Heat to 250°C and keep for 5h to obtain a pretreated elastic quartz capillary column.

[0025] Among them: the column length of the elastic quartz capillary column is 50m, the inner diameter is 0.32mm, and the film thickness is 1.0um.

[0026] (2) Accurately weigh 50 mg of bentonite, add 50 mL of toluene, and conduct ultrasonic treatment at a frequency of 35KHz. After 30 minutes, the suspension of bentonite is obtained.

[0027] (3) Use the dynamic method to sequentially coat the organic bentonite suspension from both ends of the pret...

Embodiment 2

[0033] Example 2 The preparation method of a special capillary chromatographic column for liquor detection, comprising the following steps:

[0034] (1) First rinse the inner wall of the elastic quartz capillary column with 3 mol / L HCl, then rinse the inner wall of the elastic quartz capillary column with water for 3 times, and finally install the rinsed elastic quartz capillary column on the chromatographic instrument, and purge it with nitrogen. Heated to 200°C and kept for 6 hours to obtain a pretreated elastic quartz capillary column.

[0035] Among them: the column length of the elastic quartz capillary column is 50m, the inner diameter is 0.32mm, and the film thickness is 0.5um.

[0036] (2) Accurately weigh 50 mg of bentonite, add 50 mL of toluene, and perform ultrasonic treatment at a frequency of 45KHz. After 30 minutes, the suspension of bentonite is obtained.

[0037] (3) Use the dynamic method to successively coat the organic bentonite suspension from both ends of...

Embodiment 3

[0043] Example 3 The preparation method of a special capillary chromatographic column for liquor detection, comprising the following steps:

[0044] (1) First rinse the inner wall of the elastic quartz capillary column with 2 mol / L HCl, then rinse the inner wall of the elastic quartz capillary column with water for 4 times, and finally install the rinsed elastic quartz capillary column on the chromatographic instrument, and purge it with nitrogen. Heated to 300°C and kept for 4 hours to obtain a pretreated elastic quartz capillary column.

[0045] Wherein: the column length of the elastic quartz capillary column is 100m, the inner diameter is 0.25mm, and the film thickness is 0.5um.

[0046] (2) Accurately weigh 50 mg of bentonite, add 50 mL of toluene, and conduct ultrasonic treatment at a frequency of 40KHz. After 30 minutes, the suspension of bentonite is obtained.

[0047] (3) Use the dynamic method to coat the organic bentonite suspension from both ends of the pretreated...

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Abstract

The invention relates to a preparation method of a special capillary chromatographic column for detecting Baijiu. The method comprises the following steps: (1) after leaching an inner wall of an elastic quartz capillary column with HCl and clean water, mounting the elastic quartz capillary column on a chromatography instrument; introducing nitrogen gas and blowing, and heating to obtain a pre-treated elastic quartz capillary column; (2) adding organic bentonite into toluene, and carrying out ultrasonic treatment to obtain organic bentonite turbid liquid; (3) coating two ends of the pre-treatedelastic quartz capillary column with the organic bentonite turbid liquid by adopting a dynamic method; blowing and drying through nitrogen gas to obtain a capillary chromatographic column pre-coatedwith the organic bentonite; (4) after mixing medium-polar stationary liquid and polar stationary liquid according to a ratio, dissolving in an organic solvent dichloromethane to prepare a coating solution; (5) coating and immersing, with the coating solution, the capillary chromatographic column pre-coated with the organic bentonite by adopting a static method; after statically coating, connectingthe capillary chromatographic column into a gas chromatograph instrument and carrying out chromatographic column ageing treatment to obtain the special capillary chromatographic column for detectingthe Baijiu. The production method provided by the invention is simple and has good repeatability and low cost.

Description

technical field [0001] The invention relates to a preparation method of a chromatographic column, in particular to a preparation method of a special capillary chromatographic column for liquor detection. Background technique [0002] Since the country has strengthened the supervision of food safety, with the continuous improvement of production technology and analysis technology, more and more people have learned that only knowing the skeleton aroma components in liquor cannot distinguish the subtle differences of liquor. [0003] In the analysis of the aroma components of liquor, the development and innovation of gas chromatography analysis technology in the enterprise is not enough. The initial DNP packed column can only separate a dozen main skeleton components in liquor, and the separation degree of ethyl acetate and n-propanol is not very good. it is good. With the upgrading of quality control analysis technology in the liquor industry, more accurate and comprehensive ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/50
Inventor 马金婵雷晓强王钦玥俄晓
Owner 兰州东立龙信息技术有限公司
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