Method for applying liquid chromatography-high resolution mass spectrometry to determination of methylamphetamine in human urine

Abstract

The invention relates to the field of drug detection, and discloses a method for applying liquid chromatography-high resolution mass spectrometry to determination of methylamphetamine in human urine.The method comprises the following steps: A, sample solution preparation: weighing 10.0 mL of human urine and 10.0mL of water and uniformly mixing; extraction, purification, elution and concentrationof methylamphetamine: adding 2.00mL of a sample solution in a HLB solid-phase extraction column, and abandoning effluent; orderly adding 5mL of a sodium bicarbonate-boric acid buffer solution and 5mLof water to rinse, and abandoning the effluent; enabling the air to pass through the HLB solid-phase extraction column for 3min; adding 10mL of an acetonitrile-methanol solution at the ratio of 9:1 toelute, wherein the take-off speed is 1mL / min, and collecting all effluent by using a heart-shaped bottle; rotating the heart-shaped bottle in water bath of 45 DEG C in a rotary evaporator until the heart-shaped bottle is nearly dry, and blow-drying by using nitrogen on a nitrogen evaporator; dissolving residue by using 1mL of volume-metering liquid, filtering with a membrane to obtain the samplesolution for the determination of the liquid chromatography-high resolution mass spectrometry; B, performing liquid chromatogram separation; and C, performing high-resolution mass spectrometry detection. The method disclosed by the invention has the characteristics of being accurate and convenient in detection, high in sensitivity and high in precision.

Description

technical field [0001] The invention relates to the field of drug detection, that is, a liquid chromatography-high resolution mass spectrometry method is used for the determination of methamphetamine in human urine. Background technique [0002] In the prior art, for the mensuration of methamphetamine in human urine, domestic detection method commonly used at present has gas chromatography, gas chromatography-mass spectrometry, high performance liquid chromatography etc., and the known method that adopts is GB / T 29636-2013 "Gas Chromatography, High Performance Liquid Chromatography and Gas Chromatography-Mass Spectrometry Test Methods for Methamphetamine in Suspected Drugs", the shortcomings are: 1. Gas chromatography and liquid chromatography can only quantify methamphetamine Analysis, roughly judged according to the retention time of the target peak, there is a risk of false positives, and the sensitivity is low. 2. Gas chromatography-mass spectrometry can qualitatively a...

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Problems solved by technology

[0002] In the prior art, for the mensuration of methamphetamine in human urine, domestic detection method commonly used at present has gas chromatography, gas chromatography-mass spectrometry, high performance liquid chromatography etc., and the known method that adopts is GB / T 29636-2013 "Gas Chromatography, High Performance Liquid Chromatography and Gas Chromatography-Mass Spectrometry Test Methods for Methamphetamine in Suspected Drugs", the shortcomings are: 1. Gas chromatography and liquid chromatography can only quantify methamphetamine Analysis, roughly judged according to the retention time of the target peak, there is a risk of false positives, and the sensitivity is low

2. Gas chromatography-mass spectrometry can qualitatively and quantitatively analyze methamphetamine, but it also has the disadvantage of low sensitivity, and the detection limit is 2mg / L

[0003] In short, the original detection method used for the determination of methamphetamine in human urine has a cumbersome pretreatment process and low detection sensitivity, and false positives or non-detection often occur in samples with low content

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