Method for determining content of methcathinone in sample by high performance liquid chromatography

Abstract

The invention discloses a method for determining the content of methcathinone in a sample by high performance liquid chromatography. The method includes the steps of: (1) preparation of a working solution; (2) preparation of a sample solution; (3) setting of detection conditions; and (4) determination of the methcathinone content of the sample. The method provided by the invention adopts reversed-phase chromatography isocratic elution, can complete analysis within 12 minutes, has efficient and accurate detection result, can be used for determination of the methcathinone content of the sample, and provides technical support for conviction and sentencing of judicial departments.

Description

technical field

[0001] The invention relates to the field of drug detection in the field of criminal investigation, in particular to a method for determining the content of methcathinone in a sample by using high performance liquid chromatography. Background technique

[0002] Methcathinone is a new type of drug that has appeared in recent years and is quite harmful to the human body. This hazard not only affects the physiological state of the human body, but also affects people's psychological activities, and overdose can lead to death. The abuse of methcathinone is not only harmful to the human body, but also has adverse effects on the development of society. In the 2007 version of the "Catalogue of Narcotic Drugs and Psychotropic Substances" issued by the State Food and Drug Administration, the Ministry of Public Security, and the National Health and Family Planning Commission, methcathinone was listed as a class I psychotropic drug for control.

[0003] The chemical na...

Examples

Embodiment 1

[0038] Embodiment 1: internal standard method quantitative detection

[0039] The present invention adopts the method for measuring the methcathinone content in the sample by high performance liquid chromatography, comprising the steps of:

[0040] (1) Preparation of working solution: Take the standard stock solution of methcathinone, and use the solution of internal standard substance 2-phenylethylamine with a mass concentration of 0.1 mg / mL to dilute successively to obtain a mass concentration of methcathinone of 0.5 and 0.1 respectively. , 0.05, 0.01, 0.005, 0.001, 0.0005mg / mL series of standard solutions, and keep the concentration of the internal standard solution at 0.01mg / mL.

[0041] (2) Preparation of the sample solution: Weigh about 45 mg of the sample material (the sample material in this embodiment is prepared by mixing the methcathinone standard with other substances, and the methcathinone content is 51.32wt%), Add 20mL mobile phase with a bottle-top pipette for ...

Embodiment 2

[0047] Embodiment 2: Quantitative detection by external standard method

[0048] (1) Preparation of working solution: Take methcathinone standard stock solution and dilute in sequence to form a series of standard solutions with mass concentrations of 0.5, 0.1, 0.05, 0.01, 0.005, 0.001, and 0.0005 mg / mL.

[0049](2) Preparation of the sample solution: Weigh about 45 mg of the sample material (the sample material in this embodiment is prepared by mixing the methcathinone standard with other substances, and the methcathinone content is 51.32wt%), Add 20mL mobile phase with a bottle-top pipette for extraction, shake for 10 minutes, centrifuge for 5 minutes, absorb 1mL of the supernatant with a 1mL pipette after centrifugation, add 10mL of mobile phase with a bottle-top pipette, shake evenly and take 1.5mL Install the automatic sample bottle to get the sample solution;

[0050] (3) The setting of detection condition: adopt Agilent SB-Phenyl chromatographic column, specification ...

Embodiment 3

[0055] The difference between this embodiment and Example 1 is that the sample and the sample pretreatment process are different: the sample used is 45 mg of blood with a methcathinone content of 51.32 wt%, that is, blank blood is taken, and a methcathinone standard is added; Add 17 mL of a mixed solution of anisole, dichloromethane and ether to extract the methcathinone in the sample, the volume ratio of anisole, methylene chloride and ether is 5:2:1.5, and add Add 10 mL of hydrochloric acid with a mass fraction of 15% HCl, remove the organic phase, and place the residue on a 35°C 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 Finally, use a 1mL pipette to absorb 1mL of the supernatant, add about 0.1mg of internal standard substance 2-phenylethylamine, and add 10mL of mobile phase with a bottle-top pipette, shake evenly, take 1.5mL and put it in an auto...

technical field

[0001] The invention relates to the field of drug detection in the field of criminal investigation, in particular to a method for determining the content of methcathinone in a sample by using high performance liquid chromatography. Background technique

[0002] Methcathinone is a new type of drug that has appeared in recent years and is quite harmful to the human body. This hazard not only affects the physiological state of the human body, but also affects people's psychological activities, and overdose can lead to death. The abuse of methcathinone is not only harmful to the human body, but also has adverse effects on the development of society. In the 2007 version of the "Catalogue of Narcotic Drugs and Psychotropic Substances" issued by the State Food and Drug Administration, the Ministry of Public Security, and the National Health and Family Planning Commission, methcathinone was listed as a class I psychotropic drug for control.

[0003] The chemical na...

Examples

Embodiment 1

[0038] Embodiment 1: internal standard method quantitative detection

[0039] The present invention adopts the method for measuring the methcathinone content in the sample by high performance liquid chromatography, comprising the steps of:

[0040] (1) Preparation of working solution: Take the standard stock solution of methcathinone, and use the solution of internal standard substance 2-phenylethylamine with a mass concentration of 0.1 mg / mL to dilute successively to obtain a mass concentration of methcathinone of 0.5 and 0.1 respectively. , 0.05, 0.01, 0.005, 0.001, 0.0005mg / mL series of standard solutions, and keep the concentration of the internal standard solution at 0.01mg / mL.

[0041] (2) Preparation of the sample solution: Weigh about 45 mg of the sample material (the sample material in this embodiment is prepared by mixing the methcathinone standard with other substances, and the methcathinone content is 51.32wt%), Add 20mL mobile phase with a bottle-top pipette for ...

Embodiment 2

[0047] Embodiment 2: Quantitative detection by external standard method

[0048] (1) Preparation of working solution: Take methcathinone standard stock solution and dilute in sequence to form a series of standard solutions with mass concentrations of 0.5, 0.1, 0.05, 0.01, 0.005, 0.001, and 0.0005 mg / mL.

[0049](2) Preparation of the sample solution: Weigh about 45 mg of the sample material (the sample material in this embodiment is prepared by mixing the methcathinone standard with other substances, and the methcathinone content is 51.32wt%), Add 20mL mobile phase with a bottle-top pipette for extraction, shake for 10 minutes, centrifuge for 5 minutes, absorb 1mL of the supernatant with a 1mL pipette after centrifugation, add 10mL of mobile phase with a bottle-top pipette, shake evenly and take 1.5mL Install the automatic sample bottle to get the sample solution;

[0050] (3) The setting of detection condition: adopt Agilent SB-Phenyl chromatographic column, specification ...

Embodiment 3

[0055] The difference between this embodiment and Example 1 is that the sample and the sample pretreatment process are different: the sample used is 45 mg of blood with a methcathinone content of 51.32 wt%, that is, blank blood is taken, and a methcathinone standard is added; Add 17 mL of a mixed solution of anisole, dichloromethane and ether to extract the methcathinone in the sample, the volume ratio of anisole, methylene chloride and ether is 5:2:1.5, and add Add 10 mL of hydrochloric acid with a mass fraction of 15% HCl, remove the organic phase, and place the residue on a 35°C 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 Finally, use a 1mL pipette to absorb 1mL of the supernatant, add about 0.1mg of internal standard substance 2-phenylethylamine, and add 10mL of mobile phase with a bottle-top pipette, shake evenly, take 1.5mL and put it in an auto...

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