Method for determining content of methcathinone in sample by high performance liquid chromatography
A high-performance liquid chromatography and methcathinone technology, which is applied in the field of high-performance liquid chromatography to determine the content of methcathinone in samples, can solve the problems of reduced criminal investigation efficiency, low detection efficiency, and long detection time, and shorten Detection time, improved resolution, improved peak shape effects
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[0038] Example 1: Quantitative detection by internal standard method
[0039] The method for measuring the content of methcathinone in a sample by adopting high performance liquid chromatography in the present invention includes the following steps:
[0040] (1) Preparation of working solution: Take the standard stock solution of methcathinone and dilute it with a solution of the internal standard substance 2-phenylethylamine with a mass concentration of 0.1 mg / mL to produce methcathinone with a mass concentration of 0.5 and 0.1 respectively. , 0.05, 0.01, 0.005, 0.001, 0.0005mg / mL series of standard solutions, and maintain the concentration of the internal standard solution is 0.01mg / mL.
[0041] (2) Preparation of sample solution: Weigh about 45 mg of the sample material (the sample material of this example is prepared by mixing the methcathinone standard product with other substances, and the methcathinone content is 51.32wt%), Use a bottle-top pipette to add 20mL mobile phase ex...
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[0047] Example 2: External standard method quantitative detection
[0048] (1) Preparation of working solution; take the standard stock solution of methcathinone and sequentially dilute it into a series of standard solutions with mass concentrations of 0.5, 0.1, 0.05, 0.01, 0.005, 0.001, 0.0005 mg / mL.
[0049] (2) Preparation of sample solution: Weigh about 45 mg of the sample material (the sample material of this example is prepared by mixing the methcathinone standard product with other substances, and the methcathinone content is 51.32wt%), Use a bottle-top pipette to add 20mL of mobile phase for extraction, shake for 10 minutes, centrifuge for 5 minutes, after centrifugation, use a 1mL pipette to absorb 1mL of supernatant, use a bottle-top pipette to add 10mL of mobile phase, shake evenly and take 1.5mL Install the automatic sample injection bottle to get the sample solution;
[0050] (3) Setting of detection conditions: adopt Agilent SB-Phenyl chromatographic column, specifica...
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[0054] Example 3
[0055] The difference between this example and Example 1 lies in the sample and sample pretreatment process: the sample used is 45 mg of blood with a methcathinone content of 51.32wt%, that is, blank blood is taken and the methcathinone standard is added; Add 17 mL of a mixed solution of anisole, dichloromethane and diethyl ether to extract the methcathinone in the sample. The volume ratio of anisole, dichloromethane and diethyl ether is 5:2:1.5, and add to the separated organic phase Add 10 mL of hydrochloric acid with 15% HCl mass fraction, remove the organic phase, place the residue on a 35℃ rapid concentrator to concentrate to dryness, add 20 mL of mobile phase to extract with a bottle-top pipette, shake for 10 minutes, centrifuge for 5 minutes, and centrifuge Then use a 1mL pipette to suck up 1mL of the supernatant, add about 0.1mg of internal standard substance 2-phenethylamine, and use a bottle-top pipette to add 10mL of mobile phase. After shaking evenl...
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