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In view of the previous report of the possibility of 33'-T2 and r-T3 measurements, the identification of these iodinated compounds was performed by mass fragmentography. The peaks at m/e 218, 624 (33'-T2) and m/e 218, 750 (r-T3) were applied to establish the precise qualitative evaluation of unknown peaks. The base peak at m/e 218 (thyroid analogues) was applied to avail itself of simultaneous multiple ion analyses by GC-MS. The following results were obtained. 1) Mass fragmentography makes possible the simultaneous measurements of 33'-T2, r-T3 and other thyroid analogues with 1 ml of serum and urine samples obtained from rats or human beings. 2) This method is very convenient for extracting the compounds from biological fluids, and the procedure can be carried out easily in a short time. The specificity of this method surpasses and cannot be compared to any other existing quantitative methods.

A Simple Method for the Simultaneous Analysis of r-T3 and 33′-T2 by Mass Fragmentography using GC-MS