NP-HPLC分离氨氯地平对映体及其含量测定

建立直接拆分氨氯地平对映体的HPLC方法,并用于其含量测定.以CHIRALPAK AD-H为固定相,在正相条件下考察了流动相组成、流速、柱温等因素对氨氯地平对映体分离度的影响.在优化条件下,分别测定了氨氯地平对映体的含量.实验表明,以正己烷-乙醇-二乙胺(95 : 5 : 0.1,体积比)为流动相,流速 1.0 Ml/min,检测波长 360 nm,柱温 30 ℃,氨氯地平对映体的质量浓度均在0.01 ～0.06 g/L范围内线性关系良好(Rr=0.998 3,Rs=0.998 7).高、中、低3个浓度平均回收率(n=3)分别为99%、101%、101%,相对标准偏差依次为0.76%、0.68%、0.98%.该分析方法准确可靠、快速、简单、重复性好,可用于左旋氨氯地平工业化制备中动态拆分过程的跟踪分析及产品质量控制. 含量.实验表明,以正己烷-乙醇-二乙胺(95 : 5 : 0.1,体积比)为流动相,流速 1.0 Ml/min,检测波长 360 nm,柱温 30 ℃,氨氯地平对映体的质量浓度均在0.01 ～0.06 g/L范围内线性关系良好(r_R=0.998 3,r_S=0.998 7).高、中、低3个浓度平均 收率(n=3)分别为99%、101%、101%,相对标准偏差依次为0.76%、0.68%、0.98%.该分析方法准确可靠、快速、简单、重复性好,

NP-HPLC Separation and Determination of Amlodipine Enantiomers

To establish a NP - HPLC method for separation and determination of amlodipine enanti-omers. Influences of composition of mobile phase, flow rate, and column temperature on separation efficiency of amlodipine enantiomers were investigated and optimized by using CHIRALPAK AD-H as chiral stationary phase. The optimal conditions were as follows: mobile phase : hexane - alcohol -diethylamine (95 : 5 : 0. 1, by volume) ; flow rate: 1.0 mL/min; column temperature; 30 ℃; detection wavelength; 360 nm. Under the optimal conditions, the linear ranges of amlodipine enan-tiomers both were between 0. 01 and 0. 06 g/L, their correlative coefficients were 0.998 3 and 0. 998 7, respectively. The average recoveries of amlodipine enantiomers at high, middle and low concentrations were 99% , 101% and 101% , with RSDs of 0. 76% , 0. 68% and 0. 98% , respectively. The developed method was accurate, reliable and reproducible, and could be used for tracing and analyzing the dynamic splitter process for S-amlodipine industrialized preparation and quality con-trol of product.