论文部分内容阅读
比较标准草案和《美国药典》恩替卡韦有关物质的测定方法,确定恩替卡韦有关物质的测定方法.采用Welch uLtimate AQ-C18柱(4.6 nm×250 mm,5μm),体积流量为1.0 mL/min,柱温为30℃,检测波长为254 nm.标准草案以水-乙腈-5％三氟乙酸(95:5:0.05)为流动相A、乙腈为流动相B,进行梯度洗脱;《美国药典》以水-乙腈(97∶3)为流动相A、乙腈为流动相B,进行梯度洗脱.均采用自身对照法测定.两种方法中非对映异构体RRS、RRR、SRR,8-羟基恩替卡韦和8-羟甲基恩替卡韦分离度均符合要求.标准草案非对映异构体RRS、RRR、SRR回收率分别为98.2％,98.5％和98.6％,RSD％分别为1.4％,1.9％/和1.8％;《美国药典》非对映异构体RRS、RRR、SRR回收率分别为99.8％,98.2％和98.5％,RSD％分别为1.4％,1.7％和1.9％.标准草案灵敏度较高,分析时间较短,可用于恩替卡韦有关物质的测定.“,”To compare draft standard and USP for determination of the related substances in Entecavir,and developing the method for determination of the related substances of Entecavir,separation was carried out on a Welch uLtimate AQ-C1s (4.6 nm× 250 mm,5.0 μm),the flow rate was 1.0 mL/min at a temperature of 30 ℃.The UV detection wavelength was 254 nm.The gradient elution mobile phase consisted of two eluents:water-acetonitrile-5％ trifluoroacetic acid (95:5:0.05)as mobile phase A,acetonitrile as mobile phase B in draft standard.The gradient elution mobile phase consisted of two water-eluents:acetonitrile (97:3) as mobile phase A,acetonitrile as mobile phase B in USP.Self standard was used.The resolution of RRS、RRR、SRR、8-Hydroxy Entecavir、8-Methoxy Entecavir and entecavir was good.The recovery of the draft standard was 98.2％ (RRS) 、98.5％ (RRR) and 98.6％ (SRR),RSD％ was 1.4％ (RRS) 、1.9％ (RRR) and 1.8％ (SRR).The recovery of USP was 99.8％ (RRS) 、98.2％ (RRR) and 98.5％ (SRR),RSD％ was 1.4％ 、1.7％ and 1.9％ o The draft standard is more sensitive and quick.It can be uesd for determination of the related substances in Entecavir.