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.
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[0029] Example 1 Pretreatment
[0030] (1) Extraction: Weigh 5g of sample and mix with 20ml trichloroacetic acid aqueous solution (5wt%), homogenize for 3min (10000r / min), centrifuge for 5min (5000r / min), collect the supernatant and place it in a 50ml volumetric flask; filter residue Mix with 20ml of trichloroacetic acid (5%), sonicate for 10min, centrifuge for 5min, combine the supernatant into a 50ml volumetric flask, and dilute with trichloroacetic acid. Take 20ml of the supernatant and mix with 20ml of n-hexane and let it stand for 3 minutes. The lower layer is the sample layer.
[0031] In view of the coarser characteristics of beef fiber, the selection of homogenized extraction method is conducive to the dissolution of biogenic amines in beef. The use of ultrasonic secondary extraction makes the dissolution of biogenic amines more thorough and reduces the loss of biogenic amines in pretreatment. Beef is rich in fat, which has a greater impact on the recovery rate. The presen...
Example Embodiment
[0044] Feasibility analysis of the method of Example 2
[0045] (1) Standard curve and detection limit
[0046] A linear test was performed with a mixed standard solution of six kinds of biogenic amines. In each single group, the concentration of each biogenic amine was 0, 0.1, 0.3, 0.5, 1.0 mg / L. Measure according to this method, use the peak area (Y) of the quantitative 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 with S / N=3 ( table 3).
[0047] Table 36 Linear relationships and detection limits of biogenic amines
[0048]
[0049] In the linear range of 0-1.0mg / L, the correlation coefficients of the linear equations of the six biogenic amines were all greater than 0.994, and the detection limit was 10μg / kg, which met the determination requirements.
[0050] (2) Accuracy and precision
[0051] The mixed standard solution was added to th...
Example Embodiment
[0056] Example 3 Determination of beef samples
[0057] The above method was used to determine the biogenic amines in beef stored at room temperature (4°C) for 7 days. 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 3.18mg / kg and 0.089mg / kg, respectively. The other four biogenic amines were basically not detected.
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