Method for qualitatively screening 242 kinds of compounds by liquid phase chromatography-mass spectra at the same times

A liquid chromatography and screening technology, applied in the field of qualitative screening of compounds, to achieve the effects of high sensitivity, fast method and strong specificity

Active Publication Date: 2009-04-01
上海市公安局刑事侦查总队
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] However, there is no effective detection method for the va

Method used

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  • Method for qualitatively screening 242 kinds of compounds by liquid phase chromatography-mass spectra at the same times
  • Method for qualitatively screening 242 kinds of compounds by liquid phase chromatography-mass spectra at the same times
  • Method for qualitatively screening 242 kinds of compounds by liquid phase chromatography-mass spectra at the same times

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1 242 kinds of compound detection

[0049] 242 compounds (drugs, poisons) and internal standards:

[0050] Paraquat, ibuprofen, methylecgonine hydrochloride, chlormequat, econine hydrochloride, iconine ethyl ester, methyldopa, dopamine hydrochloride, isoniazid, pholcodine, acyclovir, nicotine, Niacinamide, isoproterenol hydrochloride, normorphine, morphine-D 3 , Morphine, Methamidophos, Noroxymorphone, Oxymorphone, Acephate, Hydromorphone, Salbutamol, Cimetidine, Paracetamol, Phenylpropanolamine Hydrochloride, Omethoate, Cathinone, Sulpiride , theophylline, ephedrine hydrochloride, pseudoephedrine hydrochloride, methcathinone, procaine, norcodeine, dihydrocodeine tartrate, clonidine hydrochloride, naloxone hydrochloride, amyrex, methylcathinone hydrochloride Ephedrine, codeine phosphate, levamisole, racemic anisodamine, amphetamine sulfate, aminopyrine, artemisinin, scopolamine hydrobromide, oxycodone, mescaline, caffeine , Amphetamine, Naltrexone Hydrochlori...

Embodiment 2

[0370] The detection of embodiment 2 aconitine, hypoaconitine and neoaconitine

[0371] Fu Mou in Nanhui District died of poisoning after drinking homemade medicinal wine at home. Take the leftover medicinal wine for inspection.

[0372] Waters Alliance 2695 / Quattro Premier XE series quadrupole liquid-mass spectrometer (Waters, USA), equipped with MassLynxV4.1 software.

[0373] The reference substances of aconitine, hypoaconitine and neoaconitine are all from China Institute for the Control of Pharmaceutical and Biological Products

[0374] Reagents: Acetonitrile is chromatographically pure, formic acid, ammonium formate, and chloroform are analytically pure, and water is pure water.

[0375] sample handling

[0376] Take 1 mL of the leftover medicinal wine test material, extract with 5 mL of chloroform, shake for 3 min, centrifuge, remove the supernatant and dry it in a water bath at 60 ° C, and set 100 μL of the initial mobile phase (also called the equilibrium mobile ph...

Embodiment 3

[0413] In a watermelon field in Songjiang District, a case of sabotaging production and operation occurred, and a plastic bottle was extracted from the scene and sent for inspection.

[0414] In this case, the herbicide paraquat is required to be tested. There is no need for gradient elution to separate more than 200 compounds, so isocratic elution is used. The experimental conditions are as follows:

[0415] Waters Alliance 2695 / Quattro Premier XE series quadrupole liquid-mass spectrometer (Waters, USA), equipped with MassLynxV4.1 software.

[0416] The reference substance of paraquat was obtained from Shanghai Pesticide Research Institute.

[0417] Reagents: Acetonitrile is chromatographically pure, formic acid, ammonium formate, and chloroform are analytically pure, and water is pure water.

[0418] Liquid chromatography conditions: the mobile phase is acetonitrile (containing 0.05% formic acid and 5mM ammonium formate): water (containing 0.05% formic acid and 5mM ammoniu...

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Abstract

The invention discloses a method which can carry out qualitative screening to 242 compounds (drugs or toxicants) simultaneously. A mode of liquid chromatogram-mass spectrometry (LC-MS/MS) multi-reaction monitoring (MRM) is adopted to carry out determinedness to objects by two pairs of parent ion-daughter ion pair and retention time. The 242 drugs or toxicants comprise toxic products such as opioids, amphetamine and cocaines and the like, bromazepam such as benzodiazepines and barbiturates, and common drugs, alkaloid, pesticide (including organophosphates, carbamates, pyrethroid pesticide residues and organochlorine pesticide), weed killer, raticide and the like.

Description

technical field [0001] The present invention relates to a method for qualitative screening of compounds, in particular to a method for qualitative screening of multiple compounds at the same time, more specifically to a liquid chromatography-mass spectrometry (HPLC-MS) method for qualitative screening of 242 compounds at the same time LC-MS / MS) method. Background technique [0002] Liquid chromatography-mass spectrometry technology is an advanced analysis technology in the world today. Compared with other commonly used methods and technologies, it only needs simple pretreatment of samples, is efficient, fast, and sensitive, and has a high probability of analyzing mixtures. Selectivity and wide applicability are especially suitable for the analysis of samples with low content of detection targets and difficult separation of detection targets. Therefore, using liquid chromatography-mass spectrometry to analyze mixed samples can greatly shorten the analysis time, reduce the wa...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N27/64
Inventor 张玉荣梁晨叶海英汪国权汪蓉倪春芳刘耀张润生
Owner 上海市公安局刑事侦查总队
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