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Method for measuring seven kinds of organic acid in rice wine by adopting solid-phase extraction-liquid-phase chromatogram method

A solid-phase extraction column and organic acid technology, applied in the field of yellow rice wine detection, can solve the problems of poor separation, complex chemical composition, cumbersome processing process, etc., and achieve the effects of accurate method, high sensitivity and good linear correlation.

Active Publication Date: 2015-11-25
JIANGNAN UNIV
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  • Claims
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Problems solved by technology

At present, the analysis of organic acids in rice wine mainly adopts the method of direct HPLC analysis and detection after sample filtration membrane treatment, but simple filtration membrane treatment can not effectively reduce the interference of impurities on the analysis of organic acids, resulting in the analysis based on HPLC The method for detecting organic acids in rice wine has the disadvantages of poor resolution, low recovery and poor accuracy
[0004] Solid phase extraction technology is a commonly used sample pretreatment technology in analysis and detection. It plays an important role in the purification and concentration of samples. It has been reported that it will be applied to the detection of organic acids in fruit vinegar and fruit juice. Most of the application methods use anion Type solid phase extraction small column, through the adsorption of organic acids, then elute, and then collect the eluate for detection, there is a problem of cumbersome processing
At present, there is no literature or report on the application of solid phase extraction technology to the processing of yellow rice wine samples.
Moreover, the chemical composition of yellow rice wine is very complex. The protein content is about 5-7g / L, the total amino acid content is about 3-4g / L, and the polysaccharide content reaches 16.7g / L. In addition, due to the Maillard reaction, there are a lot of pigments in yellow rice wine. , the existence of these complex components will seriously interfere with the separation and analysis of organic acids

Method used

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  • Method for measuring seven kinds of organic acid in rice wine by adopting solid-phase extraction-liquid-phase chromatogram method
  • Method for measuring seven kinds of organic acid in rice wine by adopting solid-phase extraction-liquid-phase chromatogram method
  • Method for measuring seven kinds of organic acid in rice wine by adopting solid-phase extraction-liquid-phase chromatogram method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1: Detection of organic acid content in semi-dry rice wine "Shazhou Youhuang 5 Years Old"

[0054] (1) Preparation of standard samples: using mobile phase (NaH 2 PO 4 , pH=2.9) to prepare the mixed standard mother liquor of organic acids, the concentration of the mother liquor of each organic acid is oxalic acid 4.124g / L, tartaric acid 1.778g / L, malic acid 4.090g / L, lactic acid 37.314g / L, acetic acid 10.660g / L L, citric acid 4.484g / L, succinic acid 9.550g / L. When performing the linear correlation determination of organic acids, the mobile phase mixed standard mother solution is used for gradient dilution, and the concentration range of each organic acid is between 0.0001 ~ 40g / L.

[0055] (2) Solid-phase extraction purification: Take a strong cation-exchange solid-phase extraction (SCX) column with 5 mg of filler and a column volume of 3 ml, activate the column with pure methanol and ultrapure water with a column volume of 3 ml in turn, and use the mobile phas...

Embodiment 2

[0071] Example 2: Effect of solid-phase chromatographic column type on the detection of rice wine organic acids

[0072] (1) Preparation of yellow rice wine samples to be tested: take two parts of semi-dry rice wine "Shazhou Youhuang 5 Years Old", one part is added with solid powder of organic acid standard, the addition amount is 0.096g / L of oxalic acid, 0.117g / L of tartaric acid g / L, malic acid 0.249g / L, lactic acid 3.51g / L, acetic acid 0.825g / L, citric acid 0.821g / L, succinic acid 1.10g / L, mobile phase (NaH 2 PO 4 , pH2.9) was diluted 3 times for later use.

[0073] (2) Solid-phase extraction purification: Take 5 mg of filler and 3 ml of strong cationic solid-phase extraction (SCX) column, weak cationic solid-phase extraction (WCX) column, and C18 solid-phase extraction column, all using 3 ml of Pure methanol and ultrapure water activated the cartridge, and the prepared rice wine samples were sent to three different solid-phase extraction cartridges for purification treat...

Embodiment 3

[0085] Example 3: Detection of organic acid content in rice wine samples under different HPLC detection methods

[0086] (1) Preparation of yellow rice wine samples to be tested: take dry yellow rice wine "Guyue Longshan Yuanhong Wine", semi-sweet yellow rice wine "Jimo Miaofu", sweet yellow rice wine "Guyue Longshan Xiangxue Wine", and use mobile phase (NaH 2 PO 4 , pH2.9) and 5mM H 2 SO 4 The yellow rice wine sample was diluted 3 times for later use.

[0087] (2) Solid-phase extraction purification: Take a strong cationic solid-phase extraction (SCX) column with 5 mg of filler and a column volume of 3 ml, activate it with 3 ml of pure methanol and ultrapure water, and purify the solid-phase extraction column of the prepared rice wine sample For processing, the first 3 mL of filtrate was discarded, and the obtained purified solution was passed through a 0.22 or 0.45 μm microporous membrane, and used as a yellow rice wine sample for later use.

[0088] (3) High performance...

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Abstract

The invention discloses a method for measuring seven kinds of organic acid in rice wine by adopting a solid-phase extraction-liquid-phase chromatogram method and belongs to the technical field of rice wine detection. The method comprises the following steps that small positive ion solid-phase extracting columns are adopted for purifying samples to be measured, a moving-phase organic acid standard substance is adopted for carrying out preparation and treatment, before the samples are fed, a 0.22-micrometer or 0.45-micrometer filter membrane is adopted for filtering to obtain liquid to be measured. High-performance liquid chromatography detection is applicable to chromatographic columns of Xselect HSS T3(Waters) and IC PAKTM ION Exclusion types. The method can effectively eliminate interference to accurate analysis of the organic acid from impurities such as protein, amino acid, polysaccharide and pigment in a rice wine matrix, has the advantages of being high in measuring speed, high in accuracy and good in repeatability, and can be used for flavor quality control and analysis of the rice wine.

Description

technical field [0001] The invention relates to a solid-phase extraction-liquid chromatography method for determining seven organic acids in rice wine, belonging to the technical field of rice wine detection. Background technique [0002] Yellow rice wine is a traditional beverage in China. It has strong aroma, mellow taste and rich nutrition, so it is loved by people. The chemical composition of rice wine is complex, and the organic acid compounds are an important part of rice wine, which have an important impact on the flavor of rice wine. Organic acids in rice wine mainly include lactic acid, succinic acid, acetic acid, malic acid, citric acid, oxalic acid and tartaric acid. "No acid can't make wine", a proper amount of organic acid can enrich the taste of rice wine and improve the quality of rice wine. However, too high or too low organic acid content in rice wine has a negative effect on the taste of rice wine, thereby causing the quality of rice wine to decline. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N1/34
Inventor 陈双徐岩王琳
Owner JIANGNAN UNIV
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