A number of analytical approaches and methods for determination of biologically active thiol compounds have been developed , including both stationary (for example voltammetry, chronopotentiometry, polarography) and flow techniques (like liquid chromatography (LC) , gas chromatography (GC) and capillary electrophoresis (CE)) . With LC systems, there are numerous detection methods, including UV detection, mass spectrometry, and electrochemical detection. Each method has its advantages and limitations and may serve a particular need in analysis.
A Protocol for the Determination of Free Thiols (spectrophotometry)
http://v.web.umkc.edu/vanhornj/freethiol.htm
Few articles based on HPLC and spectrophotometry are added for persual.
Among the methods available for measurement of S, inductively coupled plasma atomic emission spectrometry (ICP‐AES) has been proved to be accurate and rapid.