Kadiyala Raju V S N, Kothapalli Pavan Kumar S R, Peddolla Madhava Reddy, Rajput Pradeep, Sharma Hemant Kumar, Budeti Shankar Reddy, Gandham Himabindu, Nowduri Annapurna
Aurobindo Pharma Ltd Research Centre-II, Survey No: 71 & 72, Indrakaran village, Sangareddy mandal, Medak district, 502329, Andhra Pradesh, India.
Andhra University College of Engineering, Visakhapatnam-530003, Andhra Pradesh, India.
Sci Pharm. 2013 Nov 14;82(1):117-28. doi: 10.3797/scipharm.1309-12. Print 2014 Jan-Mar.
A capillary gas chromatography method using a flame ionization detector has been developed for the trace analysis of allylamine (AA) in sevelamer hydrochloride (SVH) and sevelamer carbonate (SVC) drug substances. The method utilized a mega bore capillary column DB-CAM (30 m × 0.53 mm × 1.0 μm) with a bonded and cross-linked, base-deactivated polyethylene glycol stationary phase and was validated for specificity, sensitivity, precision, linearity, and accuracy. The detection and quantitation limits obtained for allylamine were 2 μg/g and 6 μg/g, respectively. The method was found to be linear in the range between 6 μg/g and 148 μg/g with a correlation coefficient of 0.9990. The average recoveries obtained in SVH and SVC were 93.9% and 99.1%, respectively. The developed method was found to be robust for the determination of AA in sevelamer drug substances and also the specificity was demonstrated with a gas chromatograph coupled with a mass spectrometer.
已开发出一种使用火焰离子化检测器的毛细管气相色谱法，用于盐酸司维拉姆（SVH）和碳酸司维拉姆（SVC）原料药中烯丙胺（AA）的痕量分析。该方法采用大口径毛细管柱DB-CAM（30 m×0.53 mm×1.0 μm），其固定相为键合交联、碱钝化的聚乙二醇，且针对特异性、灵敏度、精密度、线性和准确度进行了验证。烯丙胺的检测限和定量限分别为2 μg/g和6 μg/g。该方法在6 μg/g至148 μg/g范围内呈线性，相关系数为0.9990。在SVH和SVC中获得的平均回收率分别为93.9%和99.1%。所开发的方法被发现对于司维拉姆原料药中AA的测定具有稳健性，并且通过气相色谱仪与质谱仪联用证明了其特异性。
