Determination of the impurity of isopentylamine hydrochloride in the intermediate of bortezomib by HPLC with pre-column derivatizationEI北大核心CSCD

A method was developed for the simultaneous determination of R-pinacol-1-amino-3-methylbutylborate hydrochloride and isopentylamine hydrochloride by pre-column derivatization high performance liquid chromatography HPLC with dichloromethane as solventtriethylamine as acid binding agent and benzoyl chloride as derivative reagent. R-pinacol-1-amino-3-methylbutylborate hydrochloride and isopentylamine hydrochloride reacted with derivatization reagent in an ice bath for 10 min. The derivatives were qualitatively determined by HPLC-mass spectrometryHPLC-MS. HPLC was performed on an AgelaVenusil MP C18 2column using methanol-water 7030V/Vas mobile phase. The flow rate was 1.0 mL/minthe detection wavelength was 236 nm and the column temperature was 35 . The UV absorption produced after derivatizationwhich could be detected by HPLC with good specificity. Isopentylamine hydrochloride derivative showed an excellent linearity in the range of 0.075-30 μµg/mLwith the limit of quantification and the limit of detectionLODof 0.075 and 0.030 μµg/mLrespectively. And the S/N of the LOQ and the LOD were 44.6 and 7.8respectively. The average recoveries were 97.7%-104.0% with the RSD of 2.9%. The method is suitable for the determination of isoamylamine hydrochloride and has significant reference value for the determination of other amine salt without UV absorption. © 2022, Youke Publishing Co.,Ltd. All rights reserved.