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Method for measuring biogenic amine in fresh chilled beef

A determination method and biogenic amine technology, applied in the field of chemical analysis, can solve the problems of complicated pretreatment, time-consuming derivatization, etc., and achieve the effects of simple and feasible method, less time, and simple and accurate detection method.

Inactive Publication Date: 2012-11-21
SHANGHAI OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a method for the determination of biogenic amines in fresh and chilled beef, which solves the problems of complicated pretreatment and time-consuming derivation in the existing biogenic amine determination methods

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  • Method for measuring biogenic amine in fresh chilled beef
  • Method for measuring biogenic amine in fresh chilled beef
  • Method for measuring biogenic amine in fresh chilled beef

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 pretreatment

[0030] (1) Extraction: Weigh 5g of the sample and mix it with 20ml of trichloroacetic acid aqueous solution (5wt%), homogenate for 3min (10000r / min), centrifuge for 5min (5000r / min), collect the supernatant and put it in a 50ml volumetric flask; Mix with 20ml of trichloroacetic acid (5%), sonicate for 10min, centrifuge for 5min, put the supernatant into a 50ml volumetric flask, and dilute to volume with trichloroacetic acid. Take 20ml of supernatant and mix with 20ml of n-hexane, let stand for 3min, the lower layer is the sample layer.

[0031] In view of the characteristics of thick beef fiber, the method of homogenate extraction is used to facilitate the dissolution of biogenic amines in beef, and the use of ultrasonic secondary extraction can make the dissolution of biogenic amines more thorough and reduce the loss of biogenic amines in pretreatment. Beef is rich in fat, which has a great influence on the recovery rate. The present invent...

Embodiment 2

[0044] The feasibility analysis of embodiment 2 method

[0045] (1) Standard curve and detection limit

[0046] The linearity test was done with the mixed standard solutions of six biogenic amines. In each single group, the concentrations of each biogenic amine were: 0, 0.1, 0.3, 0.5, 1.0 mg / L. Determined according to this method, use the peak area (Y) of the quantified ion and the corresponding standard concentration (X) as the standard curve, calculate the regression equation and correlation coefficient of the standard curve, and calculate the detection limit ( table 3).

[0047] The linear relationship and detection limit of 36 kinds of biogenic amines in table

[0048]

[0049] The correlation coefficients of the linear equations of the six biogenic amines were greater than 0.994 in the linear range of 0-1.0 mg / L, and the detection limit was 10 μg / kg, which met the determination requirements.

[0050] (2) Accuracy and precision

[0051] Add the mixed standard soluti...

Embodiment 3

[0056] Embodiment 3 Beef sample determination

[0057] Using the method above, the biogenic amines in beef stored at room temperature (4°C) for 7 days were measured, and the results are shown in Table 5.

[0058] Table 5 Biogenic amine content in beef (mg / kg)

[0059]

[0060] After the beef was stored at room temperature (4°C) for 7 days, tyramine and phenethylamine were detected at 3.18 mg / kg and 0.089 mg / kg, respectively, and the other four biogenic amines were basically not detected.

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Abstract

The invention belongs to the field of analytical chemistry, and discloses a method for measuring biogenic amine in fresh chilled beef. After the beef is extracted by trichloroacetic acid and purified by a hybrid type cationic exchange solid phase extraction column, a high efficient liquid chromatography-tandem mass spectrometer method is adopted to simultaneously measure six common biogenic amines (cadaverine, tyramine, tryptamine, putrescine, histamine, phenylethyamine) in the beef. The chromatogram part adopts a chromatographic column with hydrophilic function to perform water-methyl cyanide gradient elution; and the mass spectrum part adopts an electro-spray ion source cation model, a multi-reaction monitoring model and an external standard method to perform mass spectrum quantitative analysis. The method requires only 15min analysis time, has good linearity within the scope of 0-1.0mg / L (r>0.994), 10Mug / kg of detection lower limit, 82.4%-116.7% of average recovery rate, and 5.3%-8.7% of standard deviation. The method is simple, convenient, quick and accurate to operate, and provides a convenient and quick method for the measurement of the biogenic amines in the fresh chilled beef.

Description

technical field [0001] The invention belongs to the field of chemical analysis, in particular to a method for determining six common biogenic amines in fresh and chilled beef. Background technique [0002] Beef is rich in nutrients and is one of the most popular meat products. Its high nutrition and high moisture characteristics make it an extremely perishable food. The growth and reproduction of microorganisms is the main cause of spoilage, and the spoilage products are mainly biogenic amines. [0003] Biogenic amines are a general term for a class of low-molecular nitrogen-containing organic compounds formed by decarboxylation of amino acids or amination of aldehydes and ketones, including aliphatic (putrescine, cadaverine, spermine, spermidine, etc.), aromatic (tyramine, phenethylamine, etc.) and heterocyclic groups (histamine, tryptamine, etc.). The chemical structures of eight common biogenic amines are shown below. [0004] [0005] Trace biogenic amines are norm...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 欧杰徐晓瑾王婧
Owner SHANGHAI OCEAN UNIV
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