No abstract

Qualitative infrared spectra in the solid phase of crystalline sodium penicillins G, F, X, K, and amyl are presented as a basis for quantitative analysis. Suitable analytical infrared absorption frequencies are listed. The details of an analysis in the solid phase, with an accuracy of ± 2.0 %, for crystalline sodium penicillin G are given. Spectroscopic SHORTLY after Fleming's discovery of penicillin it was evident that because of its instability and other chemical properties the purification, isolation, characterization, and analysis of the antibiotic would not be an easy task. As purification of the material progressed it was soon found that a multiplicity of types of penicillin was produced by the mold, each type possessing its own specific antibiotic activity and properties. Because of these

U uring the first phases of the work reported herein erratic and nonreproducible results were obtained. Modification of the apparatus was necessary to obtain the final results given in Tables I and II. The data, obtained at pressures of 20, 50, 100, and 300 mm. of mercury, were plotted on x-y and f-x diagrams and smooth curves were drawn. The "visually smoothed" data are reported in Tables III and IV. Activity coefficients for both components were also calculated and included in Tables III and IV. They indicate that the systems are ideal.

A discussion is presented of the use of the Norelco Geiger counter x-ray spectrometer in the quantitative analysis of organic systems. Complete details covering certain improvements to the spectrometer and in the methods used for analysis are given. In particular, a method for the determination of the crystalline content of sodium penicillin G samples, accurate to =*"2.5%, is given.

A method has been developed using reliable GC derivatization techniques interfaced with a high resolution mass spectrometer. The method has proved successful for the detection of low levels (less than 1 ppm) of clenbuterol in complex biological matrices. Selected ion recording of two characteristic isotopic fragment ions provides a specific mode of detection by verifying the GC retention time of these ions and also by comparing their relative abundance. Analysis of urine samples demands higher mass spectrometric resolution, and 40 000 (10% valley) was found to be a prerequisite for accurate integration of the drug-related chromatographic peaks. The method developed is suitable for adaptation to a completely unattended automated routine incorporating sample injection, storage and retrieval of source tuning parameters, and data processing.