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Determination of cyanide, in urine and gastric content, by electrospray ionization tandem mass spectrometry after direct flow injection of dicyanogold.

Analytica chimica acta (2009-09-08)
Kayoko Minakata, Hideki Nozawa, Kunio Gonmori, Masako Suzuki, Osamu Suzuki
ABSTRACT

A rapid and sensitive electrospray ionization tandem mass spectrometric (ESI-MS-MS) procedure was developed for the determination of cyanide (CN(-)). CN(-) in biological fluids was reacted with NaAuCl(4) to produce dicyanogold, Au(CN)(2)(-), which was extracted with methyl isobutyl ketone (MIBK). One microliter of the extract was injected directly into an ESI-MS-MS instrument. Quantification of CN(-) was performed by selected reaction monitoring of the product ion CN(-) at m/z 26 that derived from precursor ion Au(CN)(2)(-) at m/z 249. CN(-) could be measured in the quantification range of 10(-7) to 5x10(-5) M with the limit of detection at 4x10(-8) M using 10 microL of urine within 10 min. A victim's urine and gastric content were diluted with water to 4-fold and 500-fold and measured, respectively.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
4-Methyl-2-pentanone, suitable for HPLC, ≥99.5%
Sigma-Aldrich
4-Methyl-2-pentanone, ACS reagent, ≥98.5%
Supelco
4-Methyl-2-pentanone, analytical standard
Sigma-Aldrich
2-Hexanone, reagent grade, 98%
Sigma-Aldrich
Potassium dicyanoaurate(I), 98%
Sigma-Aldrich
4-Methyl-2-pentanone, ≥99%
Sigma-Aldrich
4-Methyl-2-pentanone, ≥99%, FCC
Supelco
2-Hexanone, analytical standard
Sigma-Aldrich
Potassium dicyanoaurate(I), 99.95% trace metals basis
Supelco
2-Hexanone, analytical standard

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