Method for rapidly detecting the content of cyanide in white spirit brewing raw materials or distiller's yeast

A technology of cyanide and raw materials, which is applied in the field of liquor analysis and detection, can solve problems such as difficult application of cyanide determination, high requirements for instruments and equipment, difficulty in batching, and simple operation, so as to avoid pre-distillation treatment procedures, low requirements for instruments and equipment, and reduce The effect of matrix interference

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

As for the raw materials and koji for liquor brewing, due to the complex matrix and trace cyanide content, there is no corresponding standard analysis method for reference.
Although the current GB 5009.36-2016 "National Food Safety Standard for the Determination of Cyanide in Food" provides methods for the determination of cyanide, these methods are difficult to apply to the determination of cyanide in raw materials or the matrix of distiller's yeast
The main reason is that the pH, color and turbidity of raw materials and distiller's yeast matrix will cause serious interference to the detection of total cyanide by isonicotinic acid-pyrazolone spectrophotometry, and this spectrophotometry requires distillation pretreatment, and the required sample The amount is large, it is difficult to carry out batch and simple operation, which greatly wastes the raw materials and time of detection
However, headspace gas chromatography can be applied to the detection of liquor brewing raw materials and koji matrix without color interference, but the detection result is only the content of free cyanide, 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 the content of cyanide in white spirit brewing raw materials or distiller's yeast
  • Method for rapidly detecting the content of cyanide in white spirit brewing raw materials or distiller's yeast
  • Method for rapidly detecting the content of cyanide in white spirit brewing raw materials or distiller's yeast

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Embodiment 1 QuEChERS pretreatment of distiller's yeast

[0067] After crushing the koji pieces, pass through a 425μm standard sieve, accurately weigh 5g of koji powder into a 50mL plastic centrifuge tube, add 10mL of water to vortex and mix, soak for 30min, add 15mL of acetonitrile, ultrasonic for 15min, freeze at -20°C for 8min, put a Ceramic homogenizer, add 6.0g MgSO 4 , 1.5g NaOAc, shake and vortex immediately for 1min, then centrifuge at 5000r / min for 5min, draw (8mL) the supernatant until it contains 1200mg MgSO 4 , 400mg C 18 and 400mg GCB in a 15mL plastic centrifuge tube, vortex for 1min, centrifuge at 5000r / min for 5min, pipette 1mL of the supernatant into a 5mL EP tube, blow with nitrogen until nearly dry, add 5mL of 2g / L NaOH for colorimetric and spectroscopic analysis.

Embodiment 2

[0068] Embodiment 2 QuEChERS pretreatment of distiller's yeast

[0069] After crushing the koji pieces, pass through a 425μm standard sieve, accurately weigh 2g of koji powder into a 50mL plastic centrifuge tube, add 4mL of water to vortex and mix, soak for 15min, add 6mL of acetonitrile, sonicate for 8min, freeze at -20°C for 8min, put a Ceramic homogenizer, add 2.4g MgSO 4 , 0.6g NaOAc, shake and vortex immediately for 1min, then centrifuge at 5000r / min for 5min, draw (2mL) the supernatant to contain 300mg MgSO 4 , 100mg C 18 and 100mg 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

[0070] The mensuration of the cyanide of embodiment 3 liquor brewing koji

[0071] (1) According to the method of Example 1, QuEChERS pretreatment is carried out to Luzhou-flavored distiller's yeast (Nongqu 1), Fen-flavored distiller's yeast (Qingqu 1), and Maotai-flavored distiller's yeast (Jiangqu 1) respectively;

[0072] (2) Color development reaction: Take the samples of Luzhou-flavored koji, Fen-flavored koji, and Maotai-flavored koji treated in step (1) and transfer them to a 10mL stoppered colorimetric tube, add 2 drops of phenolphthalein indicator, and adjust with acetic acid solution. When the red color fades, adjust it to near red with 2g / L sodium hydroxide solution, then add 2mL phosphate buffer solution (if the room temperature is lower than 20°C, put it in a water bath at 25°C-30°C for 10min), then add 0.2mL chloramine T (Preparation) solution, shake well and let stand for 3min, add 2mL isonicotinic acid-barbituric acid solution, add water to the colorimetric tub...

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Abstract

The invention discloses a method for rapidly detecting the content of cyanide in white spirit brewing raw materials or distiller's yeast, and belongs to the technical field of white spirit analysis and detection. The method comprises the following steps: treating a white spirit brewing raw material or a distiller's yeast sample by adopting a QuEChERS technology, adding acetonitrile, carrying out ultrasonic treatment, adding ceramic homogeneous protons, MgSO4 and NaOAc, uniformly mixing, and carrying out centrifugal treatment; adding MgSO4, octadecylsilane chemically bonded silica C18 and graphitized carbon black GCB into the supernate, and performing centrifugal treatment after uniform mixing; finally, obtaining a white spirit brewing raw material or distiller's yeast sample subjected to QuEChERS pretreatment, and carrying out cyanide content detection by an isonicotinic acid-barbituric acid spectrophotometric method, so that the requirement on instruments and equipment is low, and rapid monitoring of wide popularization to actual production is easier to realize; and samples can be pretreated in batches, the operation is simple, and the detection efficiency can be efficiently improved. The detection method has the advantages of rapidness, economy, wide applicability and the like.

Description

technical field [0001] The invention relates to a method for rapidly detecting cyanide content in liquor brewing raw materials or koji, and belongs to the technical field of liquor analysis and detection. Background technique [0002] Cyanide refers to a class of toxic compounds with cyano groups, which are widely present in plants in the form of cyanogenic glycosides. At present, cyanides in the form of cyanogenic glycosides have been found in more than 2500 kinds of plants. After cyanide-containing plants are ingested into the human body, cyanogenic glycosides will undergo enzymatic hydrolysis in the human digestive system to generate non-glucoside cyanides (cyanohydrins and free cyanides), and the released cyanide ions can inhibit the activity of cytochrome C oxidase , Block the respiratory chain and cause tissue hypoxia, causing the body to fall into a state of internal suffocation. According to reports, the lethal dose of hydrocyanic acid taken orally by humans is 0.7-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N21/78G01N1/28
CPCG01N21/31G01N21/78G01N1/286
Inventor 陈双徐岩朱晓春
Owner JIANGNAN UNIV
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