Detection of sulphur containing compounds

Details Detection of sulphur containing compounds Detection of sulphur containing compounds

1997-02-05

1998-06-02

Alexander, Lyle A.

Chemistry: analytical and immunological testing

Sulfur containing

436172, 436120, G01N 3074

Patent

active

057598614

DESCRIPTION:

BRIEF SUMMARY
The present invention relates to a method for the detection of specific organosulphur compounds which is capable of distinguishing selected compounds from more common sulphur containing compounds eg. naturally occurring compounds such as sulphur containing amino acids. The determination of such compounds, preferably at trace levels or above, is particularly important in the fields of environmental, biological and medical analysis.
A number of liquid phase chemiluminescence procedures have been developed for the determination of inorganic and organic species mostly utilising the luminol and peroxyoxalate reactions (Robards K. and Worsfold P. J., Anal. Chim. Acta, 1992 266 147), however, other chemiluminescence reactions have been discovered, eg. certain organosulphur species have been found to give rise to chemiluminescence (Lancaster J. S. and Worsfold P. J. Anal. Proc., 1989 26 19). The present invention provides methods which are capable of distinguishing a specific group of organosulphur compounds over other organosulphur compounds such as cysteine and cystine.
The determination of sulphur mustard, bis-(2-chloroethyl)-sulphide, a toxic agent capable of being used in chemical warfare, is of particular importance, both in warfare scenarios and in order to ensure that international laws regulating the use of such agents are not being violated. Thiodiglycol is one of the principal precursors of sulphur mustard manufacture (Lundin S. J. "Verification of Dual-Use Chemicals Under the Chemical Weapons Convention: The Case of Thiodiglycol" 1991 SIPRI) and has been shown to be a major environmental breakdown product of sulphur mustard via hydrolysis (Black R. M., Clarke R. J., Read R. W. and Reid M. T. J., J. Chromatogr., 1994 662 301), as well as being present in biological samples of persons poisoned by sulphur mustard (Wils E. R. J., Hulst A. G., de Jong A. L., Verweij A. and Boter H. L., J. Anal. Tox., 1985 9 254). Thus, the ability to detect this and other hydrolysis products of sulphur mustard eg. 2-chloro-2-hydroxydiethyl sulphide, is also valuable as an indication of the clandestine use of the active agent.
The need for the reliable determination of these compounds has led to the development of a number of sophisticated instrumental methods, mostly involving the use of gas chromatography-mass spectrometry (GC-MS) or GC-MS-MS. These use various modes of ionisation for identification and quantification and particularly use the detector in the selected ion monitoring mode for screening purposes, however, derivatisation procedures are required for the analysis of thiodiglycol. Sulphur mustard and its degradation products possess poor absorptive properties and do not fluoresce in the ultraviolet or visible regions of the electromagnetic spectrum, therefore common liquid phase methods of detection have limited applications, with the need for derivatisation again often necessary. No sensitive liquid phase systems have yet been made available which provide the necessary selectivity required for the direct determination of sulphur containing compounds such as sulphur mustard and thiodiglycol.
The high toxicity of such compounds means that their detection at low levels is of particular value. The method of the invention is capable of detecting thiodiglycol present in a sample at a concentration of 0.2 .mu.g ml.sup.-1 (2.times.106M), however, the method will also be of value for the detection of organosulphur compounds present in a sample at a concentration of 1 .mu.g ml.sup.-. The method is therefore much more sensitive than the earlier method studying chemiluminescence, described by Lancaster and Worsfold, which quotes a theoretical detection limit for 2-ethylthiophenol of 4.times.10.sup.-4 M and which gives examples showing light emission below 2.times.10.sup.-2 M and very low emission below 5.times.10.sup.-3 M.
According to this invention a method for determining the presence and/or amount of at least one compound associated with bis-(2-chloroethyl)-sulphide in a sample comprises the steps of of compounds associ

REFERENCES:
Analytical Proceedings, Jan. 1989, vol. 26; Lancaster et al; `Flow Injection Determination of Organosulphur Compounds with Chemiluminescence Detection`.

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