摘要
目的建立UPLC测定注射用醋酸西曲瑞克的有关物质含量的方法。方法采用色谱柱ACQUITY UPLC CSHTM C;(2.1 mm×150 mm,1.7μm),流动相A为0.05 mol·L^(-1)高氯酸钠溶液(磷酸调节pH值至2.0),流动相B为0.05 mol·L^(-1)高氯酸钠溶液-乙腈(30∶70)(磷酸调节pH值至2.0),梯度洗脱,流速为0.2 mL·min^(-1),检测波长为226 nm,进样量为1μL。结果杂质A、B、C、D、E、F的检测浓度范围分别为0.1278~6.3904,0.1244~6.2213,0.1268~6.3408,0.1205~6.0256,0.1209~6.0473,0.1277~6.3894μg·mL^(-1),各杂质检出限约为0.04 ng,杂质B、D、E定量限约为0.12 ng,杂质A、C、F定量限约为0.13 ng,平均加样回收率分别为97.4%,95.2%,101.5%,105.3%,100.7%,97.4%,RSD分别为1.7%,3.0%,3.8%,2.4%,0.8%,2.8%(n=9)。结论本方法快速、简便、准确、专属性强,可用于注射用醋酸西曲瑞克中有关物质的定量研究。
OBJECTIVE To establish an UPLC method for determination of related substances of Cetrorelix Acetate injection.METHODS The separation was performed on ACQUITY UPLC CSHTMC;column(2.1 mm×150 mm,1.7μm),0.05 mol·L^(-1)sodium perchlorate solution(adjust the pH with phosphoric acid to 2.0)was used as mobile phase A,and 0.05 mol·L^(-1)sodium perchlorate solution-acetonitrile(30︰70)(adjust the pH with phosphoric acid to 2.0)was used as mobile phase B,with a gradient elution.Flow rate was 0.2 mL·min^(-1),the detection wavelength was 226 nm and sample volume was 1μL.RESULTS The linear ranges of impurity A,B,C,D,E and F were 0.1278-6.3904,0.1244-6.2213,0.1268-6.3408,0.1205-6.0256,0.1209-6.0473,0.1277-6.3894μg·mL^(-1),respectively.The limits of detection of each impurities was about 0.04 ng.The limits of quantitation of impurity B,D,E were about 0.12 ng,that of impurity A,C,F were about 0.13 ng.The average recoveries were 97.4%,95.2%,101.5%,105.3%,100.7%,97.4%,respectively.RSDs were 1.7%,3.0%,3.8%,2.4%,0.8%,2.8%(n=9),respectively.CONCLUSION The method is rapid,simple,accurate and specific and can be used for the quantitative study on related substances in Cetrorelix Acetate for injection.
作者
薛巧如
刘冰滢
陈华
邓锋
XUE Qiaoru;LIU Bingying;CHEN Hua;DENG Feng(Guangdong Institute for Drug Control,NMPA Key Laboratory of Quality Control of Blood Products,Guangdong Drug Administration Key Laboratory of Quality Control and Research of Blood Products,Guangzhou 510663,China)
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2022年第2期203-207,共5页
Chinese Journal of Modern Applied Pharmacy
作者简介
薛巧如,女,硕士,副主任药师,E-mail:12236008@qq.com;通讯作者:陈华,女,硕士,主任药师,E-mail:gdchenhua@sina.com
