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

A technology of LC-MS and analytical methods, applied in analytical materials, measuring devices, material separation, etc., can solve the problems of inability to meet the needs of case inspection, large polarity, difficulty in extraction and detection, etc., to simplify experimental steps and save money. Analyzing the effect of time

Inactive Publication Date: 2010-08-25
上海市公安局刑事侦查总队
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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
Existing literature reports on the analysis of morphine alkaloids in biological s

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

Example 1

Detection of 3-β-D-glucuronomorphine, morphine, O6-monoacetylmorphine and codeine in urine samples

1. Liquid chromatography conditions

Chromatographic column: XterraMSC183.5μm2.1×150mm (Waters Company)

Mobile phase is A and B, and wherein A is the water containing 2mmol / L ammonium formate and 0.05% (v / v) formic acid, B is the acetonitrile containing 2mmol / L ammonium formate and 0.05% (v / v) formic acid, A, The volume ratio of B is 90:10.

Column temperature: 45°C

Flow rate: 0.2mL / min

Injection volume: 10μL

Example 2

Detection method: multiple reaction monitoring (MRM)

Scanning method: Positive ion scanning

Electrospray voltage: 3200V

Nebulizing gas flow rate: N2600L / hr

Cone back blowing air flow rate: N250L / hr

Ion source temperature: 105°C

Collision gas: argon

Internal standard: Morphine-d3

3. MRM parameters

For each compound, two parent ion-product ion pairs were selected, combined with retention time for qualitative determination and p...

Example Embodiment

Example 2

Detection of 3-β-D-glucuronomorphine, morphine, O6-monoacetylmorphine and codeine in urine samples

1. Liquid chromatography conditions, mass spectrometry conditions, and MRM parameters are the same as in Example 1.

Example 2

Activate the oasisHLB column (1cc / 30mg) with 1mL of methanol and 1mL of water in turn, accurately draw 1.0 urine sample, add 100ng of internal standard, mix well and put on the column, rinse the column with 1mL of water containing 5% (v / v) methanol, Then use 1mL methanol to elute, and the flow rate in the whole process is controlled at about 2mL / min. The eluate was blown dry in a water bath at 60°C under air flow, and the residue was dissolved in 100 μL of the initial mobile phase, and transferred to an autosampler vial for injection.

3. Result analysis

1) Chromatographic behavior

The retention times of 3-β-D morphine glucuronide, morphine, O6-monoacetylmorphine, codeine and internal standard are 1.98min, 2.25min, 3.58min and 4.70min re...

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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

LC-MS / MS method for detecting morphine alkaloids in whole blood and urine technical field 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-beta-D glucuronide morphine, morphine and O6-monoacetyl in whole blood and urine LC-MS / MS method for the analysis of morphine and codeine. Background technique 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...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06
Inventor 张玉荣梁晨叶海英汪蓉
Owner 上海市公安局刑事侦查总队
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