US 4,565,787 AGranted

High performance liquid chromatography (HPLC) analysis of sulfur mustards and their decomposition by-products by derivatization

AssigneeThe United States of America as represented by the Secretary of the Army

InventorsPaul C. Bossle, John J. Martin, Emory W. Sarver, Harold Z. Sommer

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Abstract

A method for the simultaneous detection, separation and analysis by reverse hase HPLC of sulfur mustard type compounds and their major hydrolysis and oxidation by-products utilizes a novel precolumn enhancement derivatization procedure. The method involves the reaction of these nonchromophoric sulfides with N-halogeno-N-metal arylsulfonamidates on a microscale to produce UV or visible absorbing or fluorescing arylsulfonylsulfilimine compounds. These arylsulfonylsulfilimine derivatives can then be readily separated on a low polarity C-18 column by reverse phase HPLC. The method permits quantitation of these sulfides by UV detector response in quantities as small as 20 nanograms.

Claims10

Dependent claims

A method for the simultaneous detection, separation, and analysis of a mixture of non-chromophoric aliphatic sulfides, which comprises:

reacting a mixture of said aliphatic sulfides of the formula R.sup.1 --S--R.sup.2, wherein R.sup.1 and R.sup.2 are alkyl radicals, which may or may not contain substituents and may be the same or different, with an alkali metal arylsulfochloramide of the formula aryl-SO.sub.2 NMeCl, wherein Me is an alkali metal, to produce a mixture of corresponding ultraviolet fluorescent arylsulfonylsulfilimine compounds according the the following equation:
##STR6## wherein Me, R.sup.1 and R.sup.2 have the aforesaid definitions;
separating the mixture of arylsulfonylsulfilimine compounds into the individual compounds by high pressure liquid chromatography (HPLC) and
fluorescing the individual arylsulfonylsulfilimines by ultraviolet radiation.

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Dependencies are inferred from the claim text.