LC-MS/MS analysis method for detecting morphinane alkaloid in whole blood and urine

Abstract

The invention discloses an LC-MS / MS analysis method for detecting morphinane alkaloid in whole blood and urine. The conditions of LC-MS and MS are separately as follows: 1) LC-MS chromatographic conditions: the mobile phase is composed of A and B, wherein A is an aqueous solution containing 2mmol / L of ammonium formate and 0.05% (v / v) of formic acid, B is acetonitrile containing 2mmol / L of ammonium formate and 0.05% (v / v) of formic acid, the volume ratio of A to B is 90:10; the column temperature is 45 DEG C; the flow rate is 0.2mL / min; the sampling volume is 10mu L; and 2) MS conditions: the detection mode adopts multiple reaction monitoring (MRM); the scanning mode adopts positive ion scanning; the electrospray voltage is 3200V; the atomization air flow rate is N2 600L / hr; the cone gas glow is N2 50L / hr; the ion source temperature is 105 DEG C; the collision gas is argon; and the internal standard adopts morphine-d3. The morphinane alkaloid contains morphine-3-beta-D-glucuronide, morphine, O6-monoacetylmorphine and codeine. The analysis method of the invention adopts solid phase extraction to purify the sample, thus the qualitative and quantitative measurements become more accurate; by adopting different elution and elution conditions, the obtained rate of recovery can be the optimal; and after the sample is added, methanol is used for further elution, thus simplifying the experimental procedures and reducing the analysis time.

Description

technical field [0001] The invention relates to an LC-MS / MS analysis method for detecting morphine alkaloids in whole blood and urine, in particular to a method for detecting 3-β-D glucuronide morphine, morphine, O 6 - LC-MS / MS method for the analysis of monoacetylmorphine and codeine. Background technique [0002] As the international drug tide continues to spread, foreign drugs are increasingly invading our country, and more and more people are taking or injecting heroin. Therefore, the requirements for the analysis and detection of morphine alkaloids in the human body are also getting higher and higher. In accordance with the Ministry of Public Security's "Definition of Drug Addiction Standards for Persons Who Take and Inject Drugs", all drug users who are seized and injected should undergo a forensic appraisal of drug addiction and identification of illegal drug use. Among them, the first element of these two identifications is the need to first test the blood or urine ...

AI Technical Summary

Problems solved by technology

Due to the strong water solubility and high polarity of the 3-β-D glucuronide morphine, it is difficult to extract and detect, so there are few reports in the literature

[0003] Existing literature reports on the analysis of morphine alkaloids in biological samples by GC-MS must undergo steps such as solvent extraction and derivatization, and cannot detect the conjugates of morphine and glucuronic acid in biological samples- 3-beta-D glucuronide morphine, therefore does not meet the needs of the case test

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