Detection of TBSA was attempted in pleural aspirates of 74 patients with tuberculous and 44 patients with nontuberculous pleural effusion by gas chromatography/mass spectrometry with selected ion monitoring. The results were disappointing with a test sensitivity of 67.6 percent and a specificity of 52.3 percent. In contrast, histologic examination of pleural biopsies gave a diagnostic sensitivity of 71.0 percent. Pleural biopsy remains a better investigational procedure for the diagnosis of tuberculous pleural effusion. Detection of TBSA was attempted in pleural aspirates of 74 patients with tuberculous and 44 patients with nontuberculous pleural effusion by gas chromatography/mass spectrometry with selected ion monitoring. The results were disappointing with a test sensitivity of 67.6 percent and a specificity of 52.3 percent. In contrast, histologic examination of pleural biopsies gave a diagnostic sensitivity of 71.0 percent. Pleural biopsy remains a better investigational procedure for the diagnosis of tuberculous pleural effusion.