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

An LC-MS and analytical method technology, 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, and save analysis time and simplify The effect of the experimental procedure

Inactive Publication Date: 2012-11-14
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
[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

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

Embodiment 1

[0043] 3-β-D glucuronate morphine, morphine, O 6 - Detection of monoacetylmorphine, codeine

[0044] 1. Liquid chromatography conditions

[0045] Column: Xterra MSC 18 3.5μm 2.1×150mm (Waters Company)

[0046] 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.

[0047] Column temperature: 45°C

[0048] Flow rate: 0.2mL / min

[0049] Injection volume: 10μL

[0050] 2. Mass Spectrometry Conditions

[0051] Detection method: multiple reaction monitoring (MRM)

[0052] Scanning method: Positive ion scanning

[0053] Electrospray voltage: 3200V

[0054] Nebulizing gas flow rate: N 2 600L / hr

[0055] Taper hole blowback flow rate: N 2 50L / hr

[0056] Ion source temperature: 105°C

[0057] Collision gas: argon

[0058] Internal standard: Morphine-d3

[0059] 3. MRM parameters

...

Embodiment 2

[0077] 3-β-D glucuronomorphine, morphine, O 6 - Detection of monoacetylmorphine, codeine

[0078] 1. Liquid chromatography conditions, mass spectrometry conditions, and MRM parameters are the same as in Example 1.

[0079] 2. Sample Processing

[0080] Activate the oasis HLB column (1cc / 30mg) with 1mL methanol and 1mL water in sequence, accurately draw 1.0 urine sample, add internal standard 100ng, mix well and put on the column, rinse the column with 1mL water containing 5% (v / v) methanol , and then eluted with 1mL of methanol, the flow rate of the whole process was 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.

[0081] 3. Result analysis

[0082] 1) Chromatographic behavior

[0083] 3-β-D Glucuronate Morphine, Morphine, O 6 - The retention times of monoacetylmorphine, codeine and internal standard und...

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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

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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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