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Method for rapidly detecting content of cyanide in baijiu brewing fermented grains

A detection method and cyanide technology, applied in the field of liquor analysis and detection, can solve the problems of difficult pre-treatment, difficult to popularize and apply, and high requirements for instruments and equipment, so as to overcome pH interference and color interference, and avoid distillation pre-treatment procedures, instruments and equipment less demanding effect

Active Publication Date: 2021-12-31
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the fermented grains of liquor brewing, because the fermented grains have high acidity and high water content, and contain complex microbial metabolites, there is currently no corresponding national standard analysis method in this field for reference
When the classic isonicotinic acid-pyrazolone spectrophotometric method recommended by the national standard is used to detect the total cyanide content in wine grains, due to the characteristics of low pH, high water content, dark color and complex components of wine grains, it is difficult to Difficult to deal with, causing serious interference to spectral detection, making accurate detection impossible; and spectrophotometry generally requires classic distillation and decolorization, which will result in a large amount of wine grains required for pre-treatment, and it is difficult to perform batch operations. The reagents cannot be stored stably, which leads to waste and cumbersome detection process
However, the headspace gas chromatography method can be applied to the detection of wine grains without color interference, but the detection result is only the content of free cyanide in wine grains, and this method requires high equipment and equipment, so it is difficult to be widely used. Popularization and application, it is difficult to meet the simple and fast detection needs in actual production

Method used

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  • Method for rapidly detecting content of cyanide in baijiu brewing fermented grains
  • Method for rapidly detecting content of cyanide in baijiu brewing fermented grains
  • Method for rapidly detecting content of cyanide in baijiu brewing fermented grains

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Embodiment 1

[0045] Embodiment 1 The method of using QuEChERS pretreatment technology to process liquor fermented grains sample

[0046] Accurately weigh 3 g of wine grains (respectively, Luzhou-flavor wine grains, Qing-flavor wine grains, and Maotai-flavor wine grains) into a 50 mL plastic centrifuge tube, add 7.5 mL of phosphate buffer (pH=9.0) and vortex to mix, soak for 15 minutes, Add 10mL acetonitrile, sonicate for 10min, freeze at -20°C for 8min, put a ceramic homogeneous ion, add 4.0g MgSO 4 , 1.0g NaCl, shake and vortex immediately for 1min, then centrifuge at 5000r / min for 5min, draw (6mL) the supernatant until it contains 750mg MgSO 4 , 120mg C 18 , 120mg NH 2 , 20mg GCB in a 15mL plastic centrifuge tube, vortex for 1min, centrifuge at 5000r / min for 5min, pipette 1mL supernatant into a 5mL EP tube, blow with nitrogen until nearly dry, add 5mL 2g / L NaOH for colorimetric and spectroscopic analysis.

Embodiment 2

[0047] Embodiment 2 The method of using QuEChERS pretreatment technology to process liquor fermented grains sample

[0048] Accurately weigh 6g of fermented grains into a 50mL plastic centrifuge tube, add 15mL of phosphate buffer (pH=8.5) and vortex to mix, soak for 30min, add 20mL of acetonitrile, ultrasonicate for 15min, freeze at -20°C for 8min, put a ceramic Homogeneous, add 8.0gMgSO 4 , 2g NaCl, shake and vortex immediately for 1min, then centrifuge at 5000r / min for 5min, draw (10mL) the supernatant until it contains 1250mg MgSO 4 , 200mg C 18 , 200mg NH 2 , 33mg GCB in a 15mL plastic centrifuge tube, vortex for 1min, centrifuge at 5000r / min for 5min, pipette 1mL supernatant into a 5mL EP tube, blow with nitrogen until nearly dry, add 5mL 2g / L NaOH for colorimetric and spectroscopic analysis.

Embodiment 3

[0050] A method for detecting cyanide content in liquor fermented grains. Using the QuEChERS pretreatment technology to process the liquor fermented grains sample, the isonicotinic acid-barbituric acid spectrophotometric method is used for detection. The specific steps of the method include the following steps:

[0051] (1) Solution preparation: Use GBW(E)080115, the standard material for cyanide component analysis in water, to prepare cyanide ion standard intermediate solution (1μg / mL); sodium hydroxide solution (2g / L, 20g / L); phenolphthalein solution (10g / mL); L); Acetic acid solution (1+24): Mix acetic acid and water at a volume ratio of 1:24; Chloramine T solution (10g / L): Dissolve 1g of Chloramine T in water and dilute to 100mL. Prepare just before use; phosphate buffer (0.5M, pH=7.0), phosphate buffer (0.2M, pH=8.5-9.0); isonicotinic acid-barbituric acid reagent: weigh 2.5g of isonicotinic acid ( C 5 h 5 o 2 N) and 1.25g barbituric acid (C 4 h 4 N 2 o 3 ), add to...

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Abstract

The invention discloses a method for rapidly detecting the content of cyanide in baijiu brewing fermented grains, and belongs to the technical field of baijiu analysis and detection. The method comprises the following steps: carrying out QuEChERS pretreatment on a fermented grain sample under an alkaline buffer condition, carrying out a reaction with chloramine T, converting CN <-> into cyanogen chloride, carrying out a chromogenic reaction with isonicotinic acid-barbituric acid to generate a purple blue dye, and determining absorbance by using a spectrophotometer; and quantificationally obtaining the cyanide content in the sample by a standard curve method. The detection method established by the invention can realize low-sample-amount rapid batch sample pretreatment, is simple to operate, has low requirements on instruments and equipment, can efficiently improve the detection efficiency, and has the advantages of rapidness, economy and wide applicability.

Description

technical field [0001] The invention relates to a rapid detection method for the content of cyanide in liquor fermented grains, in particular to a method for detecting the content of cyanide in liquor fermented grains by using QuEChERS technology and using isonicotinic acid-barbituric acid spectrophotometry, which belongs to liquor Analysis and detection technology field. Background technique [0002] Cyanide is a kind of highly toxic substance. In nature, there are widely different forms of cyanide. Its toxicity depends to a large extent on the form. Ions are the most toxic. The non-toxic cyanogenic glycosides in plants and plant-derived foods are natural sources of cyanide ions. When people eat cyanogenic foods, cyanogenic glycosides will undergo enzymatic hydrolysis in the human digestive system to generate non-glucoside cyanides (cyanohydrins and free cyanides) Compounds), the released cyanide reversibly inhibits iron-containing cellular enzymes, especially cytochrome ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N21/78
CPCG01N21/31G01N21/78
Inventor 陈双徐岩朱晓春
Owner JIANGNAN UNIV
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