Identification and determination of the photodegradation impurities in melphalan hydrochloride / 中国药科大学学报

ABSTRACT

This study was aimed to identify the photodegradation impurities (PD1 and PD2) in melphalan hydrochloride and establish a method for determining PD1 and PD2.The structures of the photodegradation impurities were inferred by LC-MS/MS.The impurities were confirmed by comparing with synthesized impurities.An HILIC method was established to determine PD1 and PD2.The method was carried out on an Atlantis HILIC column(4.6 mm × 150 mm,3 μm) with the mobile phase consisting of 0.1 mol/L ammonium formate (adjusted to pH 3.0 with formic acid) and acetonitrile (13∶ 87) at the flow rate of 1.0 mL/min.The column temperature was 35 ℃.The detection wavelength was 260 nm.PD1 and PD2 were characterized as 4-amino-L-phenylalanine hydrochloride and 4-(2-chloroethyl) amino-L-phenylalanine hydrochloride,respectively.Melphalan hydrochloride,PD1 and PD2 were separated completely under the HILIC condition.The established HILIC method can be used to determine the photodegradation impurities.