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Method for detecting histamine content in fish meal

A technology for histamine and content, applied in the field of analytical chemistry, can solve the problems of cumbersome and time-consuming pretreatment operations, difficult to control the derivatization process, and unstable derivatives.

Pending Publication Date: 2021-04-20
LIAONING WELLHOPE AGRI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Derivatization is divided into pre-column derivatization and post-column derivatization. At present, pre-column derivatization is usually used. The pre-treatment operation is cumbersome and time-consuming, the derivatization process is not easy to control, and the derivatization reagents have certain disadvantages. Some derivatives are unstable, and the test results are often Instability of parallel sample results may occur

Method used

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  • Method for detecting histamine content in fish meal
  • Method for detecting histamine content in fish meal
  • Method for detecting histamine content in fish meal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] To detect the histamine content in the fishmeal sample, the steps are as follows:

[0065] (1) Weigh 996.62mg of fishmeal sample, put it in a 25mL brown volumetric flask, add 10mL of 0.25% sulfosalicylic acid solution, shake gently, the solution will completely soak the sample, continue to add 0.25% sulfosalicylic acid solution Dilute the salicylic acid solution to 25mL, ultrasonically extract for 10min, shake well every 5min in the middle, after the ultrasonication is completed, take it out and let it cool down to room temperature. Take 10 mL of the supernatant and pour it into a 50 mL centrifuge tube, centrifuge at 8000 r / min for 10 min in a centrifuge, and pass the centrifuged supernatant through a 0.22 μm microporous membrane for analysis by an automatic amino acid analyzer.

[0066] (2) Amino acid automatic analyzer determination. The chromatographic conditions are: chromatographic column: cationic separation column, 30mm×4.6mm; mobile phase: buffer A+buffer B (30...

Embodiment 2

[0069] To detect the histamine content in the fishmeal sample, the steps are as follows:

[0070] (1) Weigh 978.02mg of fishmeal sample, put it in a 25mL brown volumetric flask, add 10mL of 3% sulfosalicylic acid solution, shake gently, the solution will completely wet the sample, continue to add 3% sulfosalicylic acid solution Dilute the syringic acid solution to 25mL, ultrasonically extract for 45min, and shake well every 5min in between. After the ultrasonication is completed, take it out and let it cool down to room temperature. Take 10 mL of the supernatant and pour it into a 50 mL centrifuge tube, centrifuge at 8000 r / min for 10 min in a centrifuge, and pass the centrifuged supernatant through a 0.22 μm microporous membrane for analysis by an automatic amino acid analyzer.

[0071] (2) Amino acid automatic analyzer determination. Chromatographic conditions: chromatographic column: cation separation column, 30mm×4.6mm; mobile phase: buffer A+buffer B (30:70), the pH valu...

Embodiment 3

[0074] To detect the histamine content in the fishmeal sample, the steps are as follows:

[0075] (1) Weigh 970.47mg of fishmeal sample, put it in a 25mL brown volumetric flask, add 10mL of 1% sulfosalicylic acid solution, shake gently, the solution will completely wet the sample, continue to add 1% sulfosalicylic acid solution Dilute the syringic acid solution to 25mL, ultrasonically extract for 30min, and shake well every 5min in the middle, after the ultrasonication is completed, take it out and let it cool down to room temperature. Take 10 mL of the supernatant and pour it into a 50 mL centrifuge tube, and centrifuge at 8000 r / min for 10 min in a centrifuge. After centrifugation, the supernatant was passed through a 0.22 μm microporous membrane for analysis by an automatic amino acid analyzer.

[0076] (2) Amino acid automatic analyzer determination. Chromatographic conditions: chromatographic column: cation separation column, 30mm×4.6mm; mobile phase: buffer A+buffer B ...

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Abstract

The invention provides a ninhydrin post-column derivatization method for detecting histamine in fish meal. The ninhydrin post-column derivatization method comprises the following steps: preparing a to-be-detected sample solution, establishing a standard curve, and detecting by using an amino acid analyzer. According to the method, the histamine content is detected by utilizing a post-column derivatization method and setting the type, the pH value and related parameters of the buffer solution, and compared with a pre-column derivatization method in the prior art, the method is simple in pretreatment operation, short in detection time consumption and good in repeatability, and has a good popularization prospect.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a post-column derivatization method for detecting histamine content in fishmeal. Background technique [0002] Fishmeal is a product obtained from whole fish or divided fish after cooking, pressing, degreasing, drying, and crushing. It has high protein content and is widely used in feed production as the main feed material. The freshness of raw fish for fishmeal production is poor or due to environmental changes such as temperature and humidity during storage, there will be spoilage and deterioration, and histamine will be produced in this process. Histamine is a kind of biogenic amine, which exists in many animals and plants, and is formed by histidine under the action of decarboxylase. Histamine content is an important indicator for evaluating the freshness of fishmeal protein. Histamine is the most toxic of biogenic amines. Excessive histamine content will cause ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 史莹吴振洲张淑枝王玥李晓丽张磊赵彦刘宇彤
Owner LIAONING WELLHOPE AGRI TECH
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