HPLC测定(1S,4R)-(4-氨基环戊-2-烯基)甲醇盐酸盐中有关物质  

Determination of the Related Substances of((1S,4R)-4-aminocyclopent-2-en-1-yl)methanol hydrochloride by HPLC

作　　者：梅妙 陈明煌 MEI Miao;CHEN Ming-huang(Hangzhou Julius Pharmaceutical Co., Ltd. ,Hangzhou,Zhejiang 310051,China;Hangzhou Minsheng Binjiang Pharmaceutical Co., Ltd.,Hangzhou,Zhejiang 310051,China)

机构地区：[1]杭州珠联医药科技有限公司,浙江杭州310051 [2]杭州民生滨江制药有限公司,浙江杭州310051

出　　处：《浙江化工》2018年第12期45-51,共7页Zhejiang Chemical Industry

摘　　要：采用异硫氰酸苯酯将样品及其没有紫外吸收的有关物质进行柱前衍生,再使用HPLC测定。检测条件:色谱柱为Agilent XDB-C18(250 mm×4.6 mm/5μm),流动相为10 mmol KH_2PO_4(A)-乙腈(B),梯度洗脱,流速为1.0 mL/min,检测波长为204 nm,柱温为25℃,样品池温度为5℃,进样量10μL。结果:(1S,4R)-(4-氨基环戊-2-烯基)甲醇盐酸盐与有关物质(包含已知和未知杂质)能达到很好的分离。杂质A,杂质B,杂质C与(1S,4R)-(4-氨基环戊-2-烯基)甲醇盐酸盐分别在0.04538～1.3614μg/mL (r^2=0.9999),0.1532～2.7039μg/mL (r^2=0.9993),0.1814～2.7210μg/mL (r^2=0.9997)和0.05161～0.9108μg/mL (r^2=0.9998)浓度内线性关系良好。杂质A、杂质B和杂质C准确度的回收率均在50%～150%范围内,且在精密度实验中,加样回收率的RSD分别为0.74%,5.75%,3.26%(n=6)。该方法准确可靠,重现性好,专属性强,可作为(1S,4R)-(4-氨基环戊-2-烯基)甲醇盐酸盐中有关物质检测的方法。The samples and their related materials were derivatized with phenyl isothiocyanate and determined by HPLC.The condition of detection were:Agilent XDB-C18column(250mm×4.6mm/5μm),the gradient mobile phase consisted of10mmol potassium dihydrogen phosphate(A)-acetonitrile(B),the flow rate was1.0mL/min,the UV detection wavelength was204nm,the column temperature was25℃and the sample pool temperature was5℃,the sample quantity is10μL.RESULTS:The resolution of((1S,4R)-4-aminocyclopent-2-en-1-yl)methanol hydrochloride and related substances(including known and unknown impurities)was good.The calibration curve were linear,the impurity A in range from0.04538~1.3614μg/mL(r^2=0.9999),the impurity B in range from0.1532~2.7039μg/mL(r^2=0.9993),the impurity C in range from0.1814~2.7210μg/mL(r^2=0.9997)and((1S,4R)-4-aminocyclopent-2-en-1-yl)methanol hydrochloride from0.05161~0.9108μg/mL(r2=0.9998).The recoveries for accuracy of the impurity A,the impurity B,the impurity C were in the range of50%~150%,and the RSD of recoveries were0.74%,5.75%and3.26%(n=6)respectively in the precision experiments.This method isaccurate and reliable,reproducible and strong,and can be used as the method ofmaterial detection in((1S,4R)-4-aminocyclopent-2-en-1-yl)methanol hydrochloride.

关 键 词：阿巴卡韦中间体 有关物质 异硫氰酸苯酯 柱前衍生 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]