摘要
目的建立盐酸莫西沙星原料药有关物质的HPLC测定方法。方法采用Agilent Eclipse Plus C18色谱柱(4.6mm×250mm,5μm)对有关物质A^H进行定量分析,以0.1%三乙胺溶液(用磷酸调节pH值至3.5)-乙腈(70:30)为流动相,流速1.0mL/min,检测波长293nm(检测杂质A、B、C、D、F),280nm(检测杂质G和H),243nm(检测杂质E),柱温30℃,进样量10μL。结果盐酸莫西沙星与各杂质峰及各杂质峰之间的分离度均大于1.5,杂质A^H的线性范围分别是0.153~1.534、0.506~1.517、0.252~1.510、0.393~1.474、0.486~1.458、0.153~1.526、0.095~1.426和0.160~1.602μg/mL,各杂质在线性范围内均与峰面积成良好的线性关系(r>0.99),杂质A^H的检测限分别为0.0511、0.1517、0.1006、0.1474、0.2430、0.0509、0.0285和0.0481μg/mL,定量限分别为0.1534、0.5056、0.2516、0.3932、0.4859、0.1526、0.0950和0.1602μg/mL,分别加入80%、100%和120%指标浓度的杂质考察回收率,结果各个杂质的回收率均在80%~120%范围内,定量限和回收率的RSD均符合验证要求。3批样品有关物质测定的结果显示,已知杂质的含量均低于0.1%。结论方法学验证结果显示,可作为检测盐酸莫西沙星的有关物质的方法。
Objective To establish the HPLC method for the determination of related substances in moxifloxacin hydrochloride.Methods The Agilent Eclipse Plus C18 chromatographic column(4.6 mm×250 mm,5μm)was used for quantitative analysis of related substances A to H,and the mobile phase consisted of 0.1%triethylamine(adjusted to pH 3.5 with phosphoric acid)-acetonitrile(70:30)at the flow rate of 1.0 mL/min;the detection wavelength was 293 nm(detection of impurities A,B,C,D,F)and 280 nm(detection impurities G and H)and 243 nm(detection of impurity E);the column temperature was maintained at 30℃and the injection volume was 10μL.Results The main peak and every impurity peak were separated well.The linear range of impurities A to H was 0.153~1.534,0.506~1.517,0.252~1.510,0.393~1.474,0.486~1.458,0.153~1.526,0.095~1.426,and 0.160~1.602μg/mL,and every impurity had a good linear relation.The LOD of impurity A^H were 0.0511,0.1517,0.1006,0.1474,0.2430,0.0509,0.0285,and 0.0481μg/mL,respectively.The LQDs of impurities A to H were 0.1534,0.5056,0.2516,0.3932,0.4859,0.1526,0.0950,and 0.1602μg/mL,respectively.By adding 80%,100%,and 120%impurities in the test solution,the recovery rates of each impurity were within the range of 80%~120%.The RSD of LQD and recovery rates met the verification requirements.The determination results of the three batch of samples showed that the known impurity was less than 0.1%.Conclusion Methodology validation results proved that the established determination method could be used for quality control of moxifloxacin hydrochloride.
作者
高莹
于建华
王胜
刘印
任继波
于辉
Gao Ying;Yu Jian-hua;Wang Sheng;Liu Yin;Ren Ji-bo;Yu Hui(Shandong Qidu Pharmaceutical Co.,Ltd.,Zibo 255400;Center for Disease Control and Prevention in Yantai Economic and Technological Development Zone,Yantai 264006;Shandong Drug and Food Vocational College,Zibo 255400)
出处
《中国抗生素杂志》
CAS
CSCD
2020年第5期455-462,共8页
Chinese Journal of Antibiotics
关键词
盐酸莫西沙星
有关物质
高效液相色谱法
Moxifloxacin hydrochloride
Related substances
High performance liquid chromatograph
