Method and kit for detecting 19 drugs and metabolites thereof in blood by liquid chromatography-tandem mass spectrometry
A technology of tandem mass spectrometry and liquid chromatography, applied in the field of detection of 19 kinds of drugs and their metabolites in blood by liquid chromatography tandem mass spectrometry, can solve problems such as poisoning and critical value of drugs, achieve short analysis time and simple sample processing method Ease of use and high sensitivity results
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[0131] 1. Clopidogrel: Accurately weigh 1.56 mg of the standard clopidogrel bisulfate, place it in a 2 mL cryovial, add 2 mL of methanol to dissolve and make to volume, and obtain a mother solution with a concentration of 597.8 μg / mL.
[0132] 2. Clopidogrel metabolite: add 1ml methanol to the sample bottle containing 1mg clopidogrel active metabolite derivative to dissolve, and obtain a mother solution with a concentration of 1000 μg / mL.
[0133] 3. 1-(2-pyrimidine)piperazine: Accurately weigh 5.78 mg of 1-(2-pyrimidine)piperazine standard substance into a 2 mL cryopreservation tube, add 2 mL of methanol to dissolve, and mix well to obtain a concentration of 2832 μg / mL stock solution.
[0134] 4. Tandospirone: Accurately weigh 2.13 mg of tandospirone standard substance into a 2 mL cryotube, add 2 mL of methanol to dissolve, and mix well to obtain a mother solution with a concentration of 1044 μg / mL.
[0135] 5. Mianserin: The purchased standard product has a known concentra...
Embodiment 2
[0168] This embodiment is used to illustrate a specific implementation of the preparation of the internal standard working solution:
[0169] 1. Clopidogrel-D3: Accurately weigh 1.79 mg of clopidogrel-D3 sulfate standard substance, put it in a 2 mL cryovial, add 2 mL of methanol to dissolve, and obtain a mother solution with a concentration of 687.4 µg / mL.
[0170] 2. The active metabolite derivative of clopidogrel-13C6: the purchase specification is 1 mg, the actual specification is 1.059 mg, directly add 1 mL of methanol to the sample bottle to dissolve, and obtain a mother solution with a concentration of 978.45 µg / mL.
[0171] 3. 1-(2-Pyrimidine)piperazine-D8: The specification of the standard product is 2.5 mg, directly add 1 mL of methanol to the sample bottle to dissolve, transfer to a 15 mL centrifuge tube, then add 1 mL in 4 times Dissolve in methanol and transfer the solution to a 15 mL centrifuge tube, mix well to obtain a mother solution with a concentration of 500...
Embodiment 3
[0197] This example is used to illustrate a specific implementation of sample processing and detection:
[0198] 1. First, use a pipette to mix at least three different concentrations of standard working solution 10 μL, internal standard working solution 10 μL and methanol:water mixed solution with a volume ratio of 1:1, and mix them in 1.5mL centrifuge tubes respectively. At least three standard solutions, the above standard solutions were vortexed and mixed at a speed of 2000rpm for 30s, and the above standard solutions were detected by liquid chromatography-mass spectrometry (the specific parameters are the same as S3), and the above-mentioned at least three standards were obtained. Solution, 19 kinds of drugs and their metabolites and internal standard chromatograms, take the ratio of the peak area of each substance of the above-mentioned at least three standard solutions to the peak area of the corresponding internal standard as the ordinate y of the standard curve, an...
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