Method for quickly detecting tetrodotoxin content in fish liver employing liquid-mass chromatography
A rapid determination, tetrodotoxin technology, applied in the field of chromatographic detection, to achieve the effect of good reproducibility, reliable results, and convenient operation
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Embodiment 1
[0027] The method for the rapid determination of tetrodotoxin content in fish liver by liquid chromatography-mass spectrometry provided by this embodiment comprises the following steps:
[0028] (1) Sample pretreatment
[0029] (1) The live puffer fish was killed by freezing, peeled, and the liver part was taken to be fully pulverized by a homogeneous sample maker, and 50 g of the liver sample was taken after crushing, and 15-20 g of kaolin was added, and continued to be pulverized by a homogeneous sample maker, and homogenized Crush for 10-15 minutes, then freeze in a -40°C refrigerator for 1-2 hours;
[0030] After freezing, weigh (1.00±0.01) g of the sample into a 50 mL polypropylene centrifuge tube, accurately add 5 mL of 30% ethanol aqueous solution and 5 mL of 1.0% acetic acid methanol solution, homogenize for 30-50 s, and extract by ultrasonic at 60 °C with a cell disruptor 25min, centrifuge at 8000r / min for 5min, transfer the supernatant to another clean centrifuge tu...
Embodiment 2
[0042] Embodiment 2 linear range and detection limit
[0043]Weigh the sample (1.00±0.01)g into a 50mL polypropylene centrifuge tube, add an appropriate amount of tetrodotoxin standard solution, the spiked levels are 0, 10, 20, 50, 100, 200μg / kg respectively, after standing for 0.5h, according to Embodiment 1 method, obtain the matrix spiked solution of 0, 10, 20, 50, 100, 200 μ g / kg; Take the peak area of TTX standard substance as the ordinate, and the matrix spiked solution concentration (μg / kg) as the abscissa, A standard curve was drawn and quantified by the external standard method. The results showed that TTX showed good linearity in the range of 10-200μg / kg, and the regression equation was Y=2.34e+003X, r 2 = 0.9994.
[0044] Equally weigh puffer fish liver samples (1.00 ± 0.01) g, add an appropriate amount of standard solution, so that the concentration level of TTX is 5.0, 10, 20, 30 μg / kg, 3 parallel samples at each level, carry out according to the method of Exa...
Embodiment 3
[0047] Recovery and precision
[0048] Take by weighing (1.00 ± 0.01) g of cultured negative puffer fish liver samples that do not contain TTX in 50mL polypropylene centrifuge tubes, divide them into 3 groups, 6 in each group, add an appropriate amount of standard solution, so that the concentrations of TTX in the samples are respectively 10, 15, 30, 50, 100, 200 μg / kg, analyzed by HPLC-MS / MS according to the method of Example 1. The matrix spiked calibration curve was quantified by the external standard method, and the recovery and precision data are shown in Table 3. A blank matrix was used for the recovery experiment, and the results were as follows:
[0049] Table 3 recovery rate and precision data
[0050] Added level / (μg.kg -1 )
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