A simple and rapid method for the quantitative measurement of mercaptoundecahydrododecarborate (BSH), (which presently is one of the most useful agents for Boron Neutron Capture Therapy) in human plasma was developed by using Fourier transform infrared spectroscopy. Different spacer thicknesses of the liquid sampling cell were examined and the optimal results were obtained by the 0.05 mm spacer. The subtraction of water absorbance from sample spectra resolved a B-H band at 2493 cm-1. The quantitative measurement of BSH was carried out by integration of the B-H band in the wavenumber range of 2534-2440 cm-1. However, at the lower BSH concentration range, a visual inspection of the spectrum to determine the wavenumber range was necessary so as to avoid any negative areas to be integrated. The lower limit of detection of BSH in aqueous solution and human plasma was 5 micrograms ml-1 (about 2.5 ppm of boron).