Determination of cyanide in blood by GC–MS using a new high selectivity derivatization reagent 1,2,3,3-tetramethyl-3H-indolium iodide

Water (Chromasolv ® LC-MS), methanol (Chromasolv ® LC-MS), n-hexane (Chromasolv ® LC-MS), acetone (Chromasolv ® LC-MS), sodium citrate, sodium tetraborate, pentafluorobenzyl bromide (PFB-Br, derivatization agent), potassium cyanide KCN and potassium cyanide K 13 CN (isotopic purity: 99% 13 C) were purchased from Sigma-Aldrich (Steinheim, Germany); Acetonitrile in LC-MS grade was purchased from Witko (Łódź, Poland); Phree™ Phospholipid Removal (1 mL) tubes were purchased from Phenomenex (Torrance, California, USA). Standard solutions of cyanide and internal standard (IS) isotope labelled analogue, were prepared in water at concentration of 5 mg/mL of cyanide ions. The working standard solutions of CNions (1000 and 10 000 ng/mL) and 13 CN ions (5000 ng/mL) were prepared by dilution of the stock solution with LC-MS grade water. Due to the high toxicity of potassium cyanide, all operations were carried out in a fume cupboard. The stock solution and standard solutions were stored at -20°C. Quality control (QC) samples were prepared by spiking blank blood to yield final concentration of 500 (low QC) and 1000 (high QC) ng/mL. Pentafluorobenzyl bromide was prepared in concentration of 100mM in LC-MS grade acetone. Saturated solution of sodium tetraborate (pH 9) was prepared by mixing 5 g of the salt with 50 mL of water. Biological materialDrug-free blank blood samples used for the development and validation of the method were obtained from Regional Blood Donation Center (Wrocław, Poland). The approval of the bioethics committee required has been obtained. Blank samples were screened prior to spiking to ensure that they were free from cyanide. Authentic human whole blood and urine samples were sent to our laboratory for toxicological analyses.

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Determination of cyanide in blood by GC–MS using a new high selectivity derivatization reagent 1,2,3,3-tetramethyl-3H-indolium iodide

Cited by 5 publications

References 32 publications

Spectral and theoretical analysis of derivatives of 1,2,3,3-tetramethyl-3H-indolium iodide (TMI), a highly selective derivatization reagent of cyanide, and their utility for the analysis of cyanide concentrations in beverages

Spectral and theoretical analysis of derivatives of 1,2,3,3-tetramethyl-3H-indolium iodide (TMI), a highly selective derivatization reagent of cyanide, and their utility for the analysis of cyanide concentrations in beverages

A gold coating nanoporous anodized alumina oxide membrane as the substrate for rapid surface enhanced Raman spectroscopy detection of conjugated cyanide in fingertip blood

The stability of cyanide in human biological samples. A systematic review, meta-analysis and determination of cyanide (GC-QqQ-MS/MS) in an authentic casework 7 years after fatal intoxication

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