A method for the simultaneous determination of epinephrine and its metabolites based on LC-MC/MS
A technology for epinephrine and metabolites, which is applied in the field of chemical analysis and detection, can solve the problems of small application range, low absolute recovery rate, large deviation of quantitative results, etc., and achieves good application prospects, reduced matrix effects, and strong qualitative ability.
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Embodiment 1
[0065] This embodiment provides a method for the simultaneous determination of epinephrine and its metabolites based on LC-MC / MS, specifically as follows:
[0066] (1) Extraction: Weigh 2.5g sample into a 50mL centrifuge tube, add 0.25mL 1μg / mL internal standard mixed solution (containing 40-200μg / kg epinephrine-d3, 20-200μg / kg 4-hydroxy- 3-methoxymandelic acid-d3, 80-200μg / kg 3,4-dihydroxymandelic acid-d3), then add 10mL of extraction solvent, vortex with a vortex mixer for 1min, and then centrifuge the Place the tube in an ultrasonic cleaner for ultrasonic extraction for 20 minutes or place it in a vortex shaker for 10 minutes. After the extraction, place the centrifuge tube in a high-speed refrigerated centrifuge for 10 minutes (12000r / min). After the centrifugation, the supernatant Remove and place in a clean container;
[0067] (2) Purification: Take 3mL of the supernatant directly through the PRiME HLB solid-phase extraction column into a clean glass test tube, then tak...
experiment example 1
[0091] Experimental Example 1 Example 1 Precision and Recovery Experiment
[0092] This experimental example utilizes the method of embodiment 1 to measure adrenaline and metabolites thereof in pork, pork liver, milk, chicken respectively; Details are as follows:
[0093] (1) Utilize the method of embodiment 1 to detect adrenaline and metabolites thereof in pork; Each pork sample is prepared 6 parallel samples according to the spiked concentration (low, medium, high three spiked concentrations), respectively, with standard curve Calculate the concentration of the quality control spiked sample to obtain the recovery precision (RSD) of the method, and the results are shown in Table 3;
[0094] (2) Using the method of Example 1 to detect adrenaline and its metabolites in pig liver; each pig liver sample was prepared with 6 parallel samples according to the spiked concentration (low, medium, high three spiked concentrations), to The standard curve calculates the concentration of ...
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