Method for determining squalene content of baijiu

A measurement method, the technology of the dogfish, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of large amount of organic solvent, complicated operation, high detection cost, etc.

Active Publication Date: 2015-07-22
KWEICHOW MOUTAI COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although the detection technology of squalene has been gradually developed and promoted, the content of squalene in liquor is very small, mostly ranging from hundreds of ng / L to dozens of μg / L, and its molecular weight is relatively large ( Molecular weight is 410), which is a relatively difficult to volatile organic compound, and this substance is an unsaturated triterpene, which is easily oxidized when exposed to the air for a long time
Therefore, there are certain difficulties in its qualitative and quantitative detection
And, also do not have the squalene detection method in the bibliographical information liquor in the prior art
[0004] Qualitative and quantitative detection in liquor cannot be achieved by direct sample injection, solid-phase microextraction, and stirring rod adsorption extraction. Although liquid-liquid extraction can enrich the trace substances in the test sample to a large extent, the operation is cumbersome. , the amount of organic solvent used is large, the demand for samples to be tested is large, the operation is complicated, and the detection cost is high

Method used

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  • Method for determining squalene content of baijiu
  • Method for determining squalene content of baijiu
  • Method for determining squalene content of baijiu

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Such as figure 1 , figure 2 , image 3 , Figure 4 As shown, a method for determining the content of squalene in liquor is to dilute the wine sample, then use multi-stage micro-extraction to establish a squalene standard curve, and use gas chromatography to obtain the organic phase obtained by multi-stage micro-extraction. -mass spectrometer analyzes it, and then compares it with the squalene standard curve, which specifically includes the following steps:

[0029] (1) Liquor dilution: dilute the liquor sample to be tested to 10% vol with ultrapure water boiled and cooled to room temperature, and set aside;

[0030] (2) Multi-stage extraction: according to step 1) the mass volume ratio of the diluted wine sample is 1:3, weigh sodium chloride, put the sodium chloride in the sample bottle, and then add the diluted wine sample into the sample bottle , and add the extractant of 1 / 18 diluted wine sample, tighten the bottle cap of the sample bottle, shake the sample bott...

Embodiment 2

[0036] Such as figure 1 , figure 2 , image 3 , Figure 4As shown, a method for determining the content of squalene in liquor is to dilute the wine sample, then use multi-stage micro-extraction to establish a squalene standard curve, and use gas chromatography to obtain the organic phase obtained by multi-stage micro-extraction. -mass spectrometer analyzes it, and then compares it with the squalene standard curve, which specifically includes the following steps:

[0037] (1) Liquor dilution: dilute the liquor sample to be tested to 10-20% vol with ultrapure water boiled and cooled to room temperature, and set aside;

[0038] (2) Multi-stage extraction: according to step 1) the mass volume ratio of the diluted wine sample is 1:3, weigh sodium chloride, put the sodium chloride in the sample bottle, and then add the diluted wine sample into the sample bottle , and add the extractant of 1 / 18 diluted wine sample, tighten the bottle cap of the sample bottle, shake the sample bo...

Embodiment 3

[0045] Such as figure 1 , figure 2 , image 3 , Figure 4 As shown, a method for determining the content of squalene in liquor is to dilute the wine sample, then use multi-stage micro-extraction to establish a squalene standard curve, and use gas chromatography to obtain the organic phase obtained by multi-stage micro-extraction. -mass spectrometer analyzes it, and then compares it with the squalene standard curve, which specifically includes the following steps:

[0046] (1) Liquor dilution: dilute the liquor sample to be tested to 15% vol with ultrapure water boiled and cooled to room temperature, and set aside;

[0047] (2) Multi-stage extraction: according to step 1) the mass volume ratio of the diluted wine sample is 1:3, weigh sodium chloride, put the sodium chloride in the sample bottle, and then add the diluted wine sample into the sample bottle , and add the extractant of 1 / 18 diluted wine sample, tighten the bottle cap of the sample bottle, shake the sample bott...

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Abstract

The invention relates to the technical field of detection of baijiu ingredients, in particular to a method for determining the squalene content of baijiu. According to the method, conditions such as the extraction stage number, the dilution of a liquor sample, types of organic solvents, chromatographic column selection and the like are optimized, and the method combining multistage-LIME (liquid-liquid micro-extraction) and GC-MS (gas chromatography-mass spectrometry) for determining the squalene content of baijiu is established. The method has the advantages of simplicity, convenience, accuracy, sensitivity and rapidness, the limit of detection of the squalene is 0.17 mu g / L, the limit of quantitation is 0.55 mu g / L, the determined recovery rate of the squalene in 11 types of baijiu ranges from 85.12% to 113.64%, the relative standard deviation is smaller than 13.80%, and quantitative analysis of trace triterpene with biological activity and with the content of ng / L or mu g / L level in baijiu can be realized.

Description

technical field [0001] The invention relates to the technical field of liquor component detection, in particular to a method for measuring squalene content in liquor. Background technique [0002] Squalene is a kind of triterpene with biological activity. Reddy LH et al. found that squalene has anti-cancer, anti-tumor, anti-oxidation and other biological activities (Squalene: A natural triterpene for use in disease management and therapy.Advanced drug delivery reviews, 2009, 61(15), 1412-1426), which are abundantly present in the liver of deep-sea sharks. [0003] Although the detection technology of squalene has been gradually developed and promoted, the content of squalene in liquor is very small, mostly ranging from hundreds of ng / L to dozens of μg / L, and its molecular weight is relatively large ( Molecular weight is 410), belongs to the less volatile organic matter, and this substance is unsaturated triterpene, it is easy to oxidize when exposed to the air for a long ti...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 胡光源林琳汪地强王莉
Owner KWEICHOW MOUTAI COMPANY
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