Liquid chromatography tandem mass spectrometry detection method for catecholamine and metabolite thereof based on magnetic solid-phase extraction
A catecholamine and liquid chromatography technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of reducing the ionization efficiency of mass spectrometry, quantitative interference of target objects, and affecting the flow rate of the solution, so as to reduce the matrix effect, reduce the limit of quantification, Effect of Improving Ionization Efficiency
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Embodiment 1
[0079] This embodiment provides a liquid chromatography tandem mass spectrometry detection method for catecholamines and their metabolites based on magnetic solid-phase extraction, wherein the catecholamines include dopamine (DA), norepinephrine (NE) and epinephrine (E), Metabolites of catecholamines include methoxytyramine (3-MT), metanephrine (MN) and norepinephrine (NMN).
[0080] The method includes the following steps:
[0081] 1) Preparation of test samples:
[0082] 1-1) Take 390 μL of the sample to be tested, add 10 μL of internal standard solution and 400 μL of aqueous solution to it, and mix at 1000 rpm for 2 minutes;
[0083] 1-2) Add 3 mg of magnetic solid-phase extraction filler into a clean sample tube, use 200 μL of acetonitrile to activate the filler, and use a magnetic solid-phase extraction instrument to transfer the filler to 400 μL of water for filler balance;
[0084] 1-3) Transfer the magnetic solid phase extraction filler in the product obtained in ste...
Embodiment 2
[0114] Embodiment 2 carries out experimental evaluation to detection method of the present invention
[0115] 1. Evaluation of matrix effect
[0116] In this experiment, the matrix effect was evaluated by adding the sample after treatment, that is, MF = the response of the blank matrix after extraction to the analyte / the response of the analyte in the pure solvent. Internal standard normalized MF = analyte MF / internal standard MF, when the range of internal standard normalized MF is 0.8-1.2 is acceptable. Three concentrations were selected for each analyte, and 5 samples of each concentration were used for determination. The results are shown in Table 4-Table 9, indicating that the MF of each compound is within the acceptable range.
[0117] Table 4 Internal standard normalization of E
[0118]
[0119] Table 5 Internal standard normalization of NE
[0120]
[0121] Table 6 Internal standard normalization of DA
[0122]
[0123] Table 7 Internal standard normaliz...
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