RESUMO
OBJECTIVE: To elucidate the structure of the major impurity in gemcitabine hydrochloride for injection. METHODS: HPLC-QTOF-MS was adopted to analyze the structure of this impurity based on the fragmentation behavior of gemcitabine and this impurity. The separation was performed on a ZORBAX Eclipse XDB-C18(4.6 mm×250 mm, 5 μm) column. A mixture of 10% methanol and 90% 10 mmol·L-1 ammonium acetate(pH 5.7) was used as mobile phase. Flow rate was 1.0 mL·min-1. MS was performed under positive mode with 4.0 kV capillary voltage, 65 V skimmer, 310 kPa spray pressure, 11 L·min-1 drying gas (nitrogen) flow rate, 350°C drying gas temperature and 150 V fragmentor. CONCLUSION: This study offers scientific data for studying the origin of the impurity of gemcitabine hydrochloride and improving its quality.