摘要
采用高效液相色谱-四极杆/飞行时间质谱(HPLC-QTOF/MS)建立了阿莫西林克拉维酸钾混悬剂(ACPS)中未知组分的鉴定方法,以BDS Hypersil C18(4.6 mm×250 mm,5μm)为色谱柱,以乙腈-水(0.1%甲酸)为流动相,流速为1 mL/min。比较了中国药典方法和HPLC-QTOF/MS方法的相关性;利用半制备液相色谱收集未知组分,并在HPLC-QTOF/MS体系中进行定位和确认,确定未知组分在液质体系中的出峰位置和准确分子量;筛查混合空白辅料成分,并通过与标准品比对,利用HPLC-QTOF/MS鉴定ACPS的未知组分为糖精钠。方法可为抗生素药品中未知组分的鉴定提供参考。
The identification of impurities in amoxicillin and clavulanate potassium for suspension(ACPS)was achieved by HPLC-quadrupole-time of flight/Mass spectrometry(HPLC-QTOF/MS).A BDS Hypersil C18(4.6 mm×250 mm,5μm)was used as the stationary phase and acetonitrile-water containing 0.1%formic acid was used as mobile phase with a flow rate of 1 m L/min.It was feasible to analysis the component of ACPS by comparing the correlation between the HPLC method in Ch.P 2015 and HPLC-QTOF/MS.The unknown component was prepared from the suspension to estimate the molecular weight by HPLC-QTOF/MS.Then,the m/z of the mixed excipients’components was screened and compared to the reference standard.The unknown component was identified to be saccharin sodium.The method provides an available idea for the identification of the unknown component in antibiotics.
作者
张艳梅
张含智
吕丹丹
刘浩
ZHANG Yanmei;ZHANG Hanzhi;LV Dan-dan;LIU Hao(Institute for Agri-Food Standards and Testing Technology,Shanghai Academy of Agricultural Sciences,Shanghai 201403;Laboratory of Quality and Safety Risk Assessment for Agro-food(Shanghai),China Ministry of Agriculture and Affairs,Shanghai 201403;Shanghai Institute for Food and Drug Control,Shanghai 201203)
出处
《分析试验室》
CAS
CSCD
北大核心
2020年第2期175-179,共5页
Chinese Journal of Analysis Laboratory
基金
上海市市级农口系统青年人才成长计划资助项目(沪农青字(2018)第1-35号)
上海市农业科学院学科领域建设专项(农科国推2019(匹配-32))资助。
作者简介
张艳梅,女(1987-),博士,助理研究员。研究方向:药物分析,色质谱分析,zymei0706@126.com;通信作者:刘浩,男(1968-),博士,主任药师。研究方向:抗生素药品质量分析与控制研究,liuhao@sifdc.org.cn。
