Analytical Development, Shasun Research Center, 27, Vandalur Kelambakkam Road, Keelakottaiyur, Chennai 600048, India.
J Pharm Biomed Anal. 2011 Jan 5;54(1):203-7. doi: 10.1016/j.jpba.2010.07.017. Epub 2010 Jul 29.
A sensitive and rapid ion chromatography (IC) method was developed for the low level determination of allylamine (AAM) in sevelamer (SVM) drug substances, i.e., sevelamer hydrochloride (SVH) and sevelamer carbonate (SVC). This method utilized a Dionex Ion Pack CS14 IC column, a mobile phase of 10mM methane sulfonic acid with conductivity detection. The total chromatographic run time was as short as 8 min. The various factors involved in the sample preparation such as, extraction solvent, extraction time and stirrer speed were evaluated. This method was validated as per United States Pharmacopoeia (USP) and International Conference on Harmonization (ICH) guidelines in terms of detection limit, quantitation limit, linearity, precision, accuracy, specificity and robustness. Linearity of the method was very good over the concentration range of 9-750 μg/mL with the coefficient of determination (r(2)) 0.999. The detection and quantitation limit of AAM were 2.7 and 9.0 μg/mL, respectively. The recovery data obtained for AAM were between 97% and 109%. Also, the specificity of the method was proved through IC coupled with mass spectrometer (IC-MS). The developed method was found to be robust and applied successfully to determine the content of AAM in Sevelamer bulk drugs.
建立了一种灵敏、快速的离子色谱（IC）法，用于低水平测定西维拉母（SVM）药物中的烯丙胺（AAM），即盐酸西维拉母（SVH）和碳酸西维拉母（SVC）。该方法采用 Dionex Ion Pack CS14 IC 柱，以 10mM 甲烷磺酸为流动相，采用电导率检测。总色谱运行时间短至 8 分钟。对样品制备中涉及的各种因素，如提取溶剂、提取时间和搅拌速度进行了评估。该方法按照美国药典（USP）和国际协调会议（ICH）的指南进行了验证，包括检测限、定量限、线性、精密度、准确度、特异性和稳健性。方法在 9-750μg/mL 的浓度范围内线性良好，相关系数（r(2)）为 0.999。AAM 的检测限和定量限分别为 2.7 和 9.0μg/mL。AAM 的回收率数据在 97%至 109%之间。此外，通过与质谱（IC-MS）联用证明了该方法的特异性。该方法被证明是稳健的，并成功地应用于测定西维拉母原料药中的 AAM 含量。
