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  • Identification and quantitation of xenobiotics by 1H NMR spectroscopy in poisoning cases.

Identification and quantitation of xenobiotics by 1H NMR spectroscopy in poisoning cases.

Forensic science international (2003-05-14)
M Imbenotte, N Azaroual, B Cartigny, G Vermeersch, M Lhermitte
ABSTRACT

In order to analyse a wide range of xenobiotics and their metabolites present in biological fluids, NMR spectroscopy can be used. A large variety of xenobiotics (therapeutic agents, pesticides, solvents, alcohols) can be characterized and quantitated directly, without sample preparation. NMR investigations were applied to acute poisoning cases, involving drugs such as salicylates and valproic acid (VPA). In a salicylate poisoning case, the three major metabolites of acetylsalicylic acid have been detected in crude urine, and rapid identification of lysine revealed the origin of the intoxication, namely lysine acetylsalicylate (Aspegic). Valproic acid as its glucuronide was identified in urine samples from two poisoned patients. 1H NMR was also used to identify and quantitate paraquat (Gramoxone) in urine owing to its two aromatic signals at 8.49 and 9.02 ppm, in two acutely poisoned patients (183 and 93 mg/l). An intentional poisoning case with tetrahydrofuran (THF) was also investigated. Serum and urine samples were collected. THF was characterized by its resonances at 1.90 and 3.76 ppm, and quantified at 813 and 850 mg/l in the two biological fluids, respectively. Moreover, two other compounds were detected: lactate and gamma-hydroxybutyric acid (GHB). 1H NMR spectroscopic analysis of serum samples from three poisoned patients revealed methanol in one case and ethylene glycol in the two others. Moreover, in the same spectrum, the corresponding metabolites formate and glycolate were found. Compared with the reference chromatographic or spectrophotometric methods, requiring time-consuming extraction and/or derivatization steps, NMR spectroscopy allows the determination of many exogenous and endogenous compounds, without any pre-selection of the analytes.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Tetrahydrofuran, anhydrous, contains 250 ppm BHT as inhibitor, ≥99.9%
Supelco
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Supelco
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Sigma-Aldrich
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Sigma-Aldrich
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Sigma-Aldrich
Tetrahydrofuran, ≥99.0%, contains 200-400 ppm BHT as inhibitor, ReagentPlus®
Sigma-Aldrich
Tetrahydrofuran, contains 250 ppm BHT as inhibitor, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥99.9%
Sigma-Aldrich
Tetrahydrofuran, contains 200-400 ppm BHT as inhibitor, ACS reagent, ≥99.0%
Sigma-Aldrich
Tetrahydrofuran, ACS reagent, ≥99.0%, contains 200-400 ppm BHT as inhibitor
Sigma-Aldrich
Tetrahydrofuran, inhibitor-free, suitable for HPLC, ≥99.9%