General Description
A Certified Spiking Solution
suitable for use in LC/MS or GC/MS applications for clinical toxicology, forensic analysis, or urine alchohol testing. Ethyl sulfate is a primary urinary metabolite of consumed alcohol and is indicative of recent alcohol consumption.
Synthesis
Weigh 0.1 mol of sodium monomethyl carbonate, and 400 grams of methanol solvent to form a solution; weigh 0.11 mol of diethyl sulfate, add it to the solution, at 30 ~ 120 , the pressure of 0 ~ 2MPa to keep 18 hours, the specific example is at 100 , 1MPa to keep 18 hours; the reaction is complete to obtain a solution of sodium ethyl sulfate in methanol. The reaction was completed by heating the solution at a reduced pressure of 6.0 kPa or less and 50C. After distillation and separation of the methanol, the temperature was increased from 50C to 100C and heated for 1 hour, and monomethyl carbonate, dimethyl carbonate, methyl ethyl carbonate, methanol, carbon dioxide and the like were distilled, of which methanol and carbon dioxide were produced by thermal decomposition of the monomethyl carbonate, and the amount was very small. Upon completion of the distillation and separation, the monohydrocarbonate salt of sulfuric acid of this example, i.e., sodium ethyl sulfate, was obtained. The yield was tested to be 99.5%, the moisture was 0.08%, the pH of the 1:100 aqueous solution was 6.8, the main content was 99.3% by cation chromatography, and the main content was 99.5% by anion chromatography.
Purification Methods
Recrystallise it three times from MeOH/Et2O and dry it in a vacuum. [Beilstein 1 H 326, 1 I 164, 1 III 1317, 1 IV 1325.]
