Analysis of cyanide in blood by headspace solid-phase microextraction (SPME) and capillary gas chromatography

Abstract

SummaryCyanide can be extracted from whole blood samples by headspace solid-phase microextraction (SPME) with a Carbowax/divinylbenzene-coated fiber. Dm'ing heating a vial of a whole blood sample containing cyanide and acetonitrile as internal standard (IS) at 50 ~ in the presence of Na2SO4, a Carbowax/divinylbenzene-coated SPME fiber was exposed in the headspace of the vial for 45 rain to allow adsorption of cyanide and IS. The fiber needle was then injected into a capillary gas chromatography (GC) instrument equipped with nitrogen-phosphorus detection. The headspace SPME-GC with a Supel-Q PLOT fused silica capillary column gave large peaks for cyanide and IS; almost no interfering peaks appeared. Recoveries of cyanide and IS flom human whole blood were 3.02-4.06 % and 0.21%, respectively. The calibration curve for cyanide added to human blood showed excellent linearity in the range of 0.04-4.0 pg mL-1; the detection limit was about 0.02 pg mL -1. The coefficients of intra-day and inter-day variation were not greater than 7.1 and 9.2 %. Good correlation (r 2 = 0.999) was found between the present SPME-GC method and the conventional microdiffusion colorimetric method. Data on determination of cyanide in rat blood after intraperitoneal administration are also presented.

Cryogenic oven-trapping gas chromatography for analysis of volatile organic compounds in body fluids

“…Results obtained in this laboratory by both COT-GC and headspace SPME-GC were compared for analysis of chloroform and dichloromethane [10,23], the components of solvent thinner [13,24], cyanide [15,25] and ethanol [16,26]. From the detection limits listed in Tables 2 and 3 it is clear that the sensitivity of COT-GC was more than tenfold that of headspace SPME-GC.…”

Determination of cyanide and volatile alkylnitriles in whole blood by headspace solid-phase microextraction and gas chromatography with nitrogen phosphorus detection

“…More recently, it has been carried out including a separation step coupled to a detection technique such as high performance liquid chromatography coupled to a fluorimetric detection [12] or capillary electrophoresis coupled to an ultraviolet detector [13]. Moreover, gas chromatography (GC) coupled to electron capture detector has been increasingly used following a derivatization step [14,15], headspace GC coupled to electron capture detector [16,17] or nitrogen-phosphorus detector (NPD) [18,19] and solid-phase microextraction (SPME) GC combined with NPD [19,20] or mass spectrometry [21]. Nevertheless, only a limited number of studies have been carried out for alkylnitriles determination in whole blood and to the best of our knowledge only one work deals with the simultaneous determination of cyanide and volatile alkylnitriles using headspace-GC-NPD [22].…”

Rapid determination of cyanide in human plasma and urine by gas chromatography–mass spectrometry with two-step derivatization

“…Several methods, including spectrometry [8][9][10][11], electrochemistry [12,13] and chromatography [14][15][16][17][18][19][20][21][22][23][24] have been reported for the determination of CN. Gas chromatography-mass spectrometry (GC-MS) appears most efficient because of the enormous abilities of high-resolution capillary column together with high selective detection system.…”

“…Gas chromatography-mass spectrometry (GC-MS) appears most efficient because of the enormous abilities of high-resolution capillary column together with high selective detection system. Headspace gas chromatography-mass spectrometry (HS-GC-MS) has been described for the determination of CN by the several research groups [15][16][17][18][19][20]. Most procedures involve the liberation of CN − from the samples as gaseous HCN by acidification, and the headspace gas was injected directly or transferred by solid-phase microextraction (SPME) to GC system for detection.…”