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It has been reported that dimethyl sulfate (DMS) can be degraded with sodium hydroxide solution (1 mol/L), sodium carbonate solution (1 mol/L), or ammonium hydroxide solution (1.5 mol/L). This has now been confirmed. Complete destruction of undiluted DMS or DMS in solvents miscible with water (methanol, ethanol, DMSO, DMF, acetone) or solvents partially miscible or immiscible with water (toluene, p-xylene, benzene, 1-pentanol, ethyl acetate, chloroform, carbon tetrachloride, acetonitrile) could be obtained using any of the above methods. Reaction times were 15 min after homogeneity was obtained for undiluted DMS, 15 min for solutions in methanol, ethanol, DMSO, and DMF, one hour for solutions in acetone, three hours for acetonitrile, and one day for the other solvents listed above. The final reaction mixtures were tested for mutagenicity, and when the solutions were not cytotoxic, no mutagenic response was obtained. DMS in solution was determined by a colorimetric method. The products of the reactions were found to be methanol when NaOH and Na2CO3 were used and methylamine, dimethylamine, trimethylamine, and methanol when ammonium hydroxide was used. The stability of DMS in various solvents was also determined.

Following reports that vitamin D sulfate is the major source of vitamin D activity in human milk, we investigated the presence of this compound in milk whey using a modification of techniques for the determination of vitamin D metabolites in plasma. Synthetic cholecalciferol sulfate, ergocalciferol sulfate an [3H]cholecalciferol sulfate were prepared by reacting radioactive cholecalciferol or nonradioactive cholecalciferol or ergocalciferol with sulfamic acid in pyridine. The products were purified sequentially by Sephadex LH-20 and high pressure liquid chromatography. The purified products were chromatographically homogeneous, exhibited an ultraviolet absorption spectrum identical to that of standard cholecalciferol, demonstrated a sulfonate ester linkage and upon saponification yielded the parent vitamin. Milk whey was extracted with methanol:methylene chloride (1:2 v/v) using [3H]cholecalciferol sulfate to estimate recovery of the compound. The extract was purified by chromatography on silica cartridges an reverse phase high pressure liquid chromatography and was quantitated by ultraviolet absorption (UV). Although added cholecalciferol sulfate was readily detected in human milk whey samples, no endogenous vitamin D sulfate was found (detection limit 1 ng/ml). The results indicate that vitamin D sulfate is not a major source of vitamin D activity in human milk.

Phenol and related compounds are toxic agents to which humans are exposed. Analysis of phenolic compounds may be used as an index of exposure. In this report a method for analysis of phenol, phenylglucuronide, phenylsulfate, and related mono- and dihydroxybenzenes as their propanoate esters by gas chromatography/mass spectrometry is presented. The use of this derivatization technique increases the sensitivity of the analysis by improving chromatographic performance and introducing a traceable "reporter" group into the analyte. This method has also been adapted, by using selected ion monitoring (SIM), to the quantitative analysis of phenol.

Sampling on solid adsorbents followed by thermal desorption and gas chromatography was evaluated as a simple method for the quantitative analysis of dimethyl sulphate, diethyl sulphate and ethylene oxide in the workplace environment. Tenax TA and Carbosieve S-III (for ethylene oxide) were found to be suitable adsorbents. The charged tubes can be stored at 22 degrees C for 4 days. The recovery is better than 98% (greater than 80% for ethylene oxide) in the mass range 1 ng-1 micrograms. The recovery is not dependent on air humidity. The limits of detection tested were at the lower parts per billion level.

An analytical method for the determination of dimethyl sulfate (DMS) and diethyl sulfate (DES) in air has been developed. The DMS and DES are adsorbed on silica gel, desorbed with acetone and determined by gas chromatography using a flame photometric detector. A solvent venting valve is utilized to allow the injection of a large sample volume without overloading the detector. By using this method, the minimum detectable concentrations in the atmosphere for DMS and DES, based on a 20 L air sample, are 0.04 ppm and 0.1 ppm, respectively.