3230 Adrjanowicz et al. Fig. 7 (a) Positive LC-MS full spectrum of a furosemide sample after cryomilling, (b) positive MS spectrum at the 8th minute of analysis (retention time of the main degradation product formed upon cryomilling), (c) MALDI-TOF MS spectra of the isolated Imp.1 (main degradation product formed upon cryomilling). Decamps et al. have shown that such a scenario even in the case of a material ground at room temperature is fairly impossible (10,11). The absence of mutarotation and carmelization process in cyclic sugars submitted to extensive grinding was proven by the presence of only an α-anomeric form in the milled material, while if the melting really had occurred, transformation from α- to β- pyranose would have been observed.