The potential of inductively coupled plasma mass spectrometry detection for high-performance liquid chromatography combined with accurate mass measurement of organic pharmaceutical compounds.

Quantification of unknown components in pharmaceutical, metabolic and environmental samples is an important but difficult task. Most commonly used detectors (like UV, RI or MS) require standards of each analyte for accurate quantification. Even if the chemical structure or elemental composition is known, the response from these detectors is difficult to predict with any accuracy. In inductively coupled plasma mass spectrometry (ICP-MS) compounds are atomised and ionised irrespective of the chemical structure(s) incorporating the element of interest. Liquid chromatography coupled with inductively coupled plasma mass spectrometry (LC/ICP-MS) has been shown to provide a generic detection for structurally non-correlated compounds with common elements like phosphorus and iodine. Detection of selected elements gives a better quantification of tested 'unknowns' than UV and organic mass spectrometric detection. It was shown that the ultrasonic nebuliser did not introduce any measurable dead volume and preserves the separation efficiency of the system. ICP-MS can be used in combination with many different mobile phases ranging from 0-100% organic modifier. The dynamic range was found to exceed 2.5 orders of magnitude. The application of LC/ICP-MS to pharmaceutical drugs and formulations has shown that impurities can be quantified below the 0.1 mol-% level.

Determination of ergosterol in organic dust by gas chromatography-mass spectrometry.

A gas chromatographic-mass spectrometric method was developed for the determination of ergosterol in organic dust. Samples were hydrolyzed under alkaline conditions, and the hydrolysate was extracted, purified on a silica-gel column, and subjected to derivatization. The limit of detection of the trimethylsilyl ether derivative of ergosterol was approximately 10 pg and that of the tert.-butyldimethylsilyl ether derivative was approximately 20 pg (injected amounts). House dust contained 6-45 micrograms ergosterol/g and air from a pig barn contained 0.2-0.3 ng ergosterol/liter. The proposed method can be used as a complement or alternative to microscopy and culturing for measuring fungal biomass in air-borne organic dust.