Bapatu Hanimi Reddy, Maram Ravi Kumar, Murthy R Satyanarayana
Department of Chemistry, JNT University, Kukatpally, Hyderabad, Telangana, India
Department of Chemistry, JNT University, Kukatpally, Hyderabad, Telangana, India.
J Chromatogr Sci. 2015 Oct;53(9):1432-42. doi: 10.1093/chromsci/bmv029. Epub 2015 Apr 8.
A novel, reversed-phase high-performance liquid chromatographic method was developed and validated for the determination of related substances in Plerixafor (PLX) drug substance. PLX is an immunostimulant used to mobilize hematopoietic stem cells in cancer patients. The method is efficient for estimation of all degradation and process-related impurities. The method was developed using the Phenomenex Luna L11 column using the gradient program with mobile phase A and mobile phase B, where mobile phase A consists of pH 2.0 1-heptanesulfonic acid sodium salt buffer and acetonitrile in the ratio of 80:20 (v/v) and mobile phase B consists of pH 2.0 1-heptanesulfonic acid sodium salt buffer and acetonitrile in the ratio of 20:80 (v/v). PLX and its impurities were monitored at 210 nm. The present work is describing the role of ion-pair reagent in the separation of polar compounds. PLX was subjected to various stress conditions of oxidative, acid, base, hydrolytic, thermal, humidity and photolytic degradations. The degradation products were well separated from each other and with the main peak, demonstrating the stability-indicating power of the method. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, ruggedness and robustness.
开发并验证了一种新型反相高效液相色谱法，用于测定普乐沙福（PLX）原料药中的有关物质。PLX是一种免疫刺激剂，用于动员癌症患者体内的造血干细胞。该方法可有效评估所有降解杂质和工艺相关杂质。该方法采用菲罗门Luna L11色谱柱，使用流动相A和流动相B的梯度程序，其中流动相A由pH 2.0的1-庚烷磺酸钠盐缓冲液和乙腈按80:20（v/v）的比例组成，流动相B由pH 2.0的1-庚烷磺酸钠盐缓冲液和乙腈按20:80（v/v）的比例组成。在210 nm波长处监测PLX及其杂质。本研究描述了离子对试剂在极性化合物分离中的作用。PLX经受了氧化、酸、碱、水解、热、湿度和光解等各种强制降解条件。降解产物彼此之间以及与主峰均得到了很好的分离，证明了该方法的稳定性指示能力。该方法的性能根据现行ICH指南进行了特异性、检测限、定量限、线性、准确度、精密度、耐用性和稳健性的验证。
