摘要
建立了贝米肝素钠中苄基三甲基氢氧化铵残留的HPLC检测方法。色谱条件为:Agilent ZORBAX Eclipse XDB-CN色谱柱(250×4.6 mm,5μm),柱温35℃,流动相为0.2 mol/L高氯酸钠水溶液(1 mol·L^(-1)高氯酸调pH=2.2)-乙腈(88∶12),流速为0.8 mL/min,检测波长为207 nm,进样量为50μL。结果表明,苄基三甲基氢氧化铵质量浓度在0.01~1.0μg/mL范围内与峰面积线性关系良好(r=0.9998,n=7);重复性试验结果的RSD为1.21%(n=6);中间精密度试验结果的RSD为1.35%(n=12);耐用性试验结果的RSD为1.20%(n=16);48 h内溶液稳定性良好,RSD为0.19%(n=13);平均加标回收率为102.40%,RSD为1.70%(n=9)。该方法操作简便、灵敏度高、结果准确可靠,可用于贝米肝素钠中苄基三甲基氢氧化铵残留的测定。
An HPLC method for determination of Benzyltrimethylammonium hydroxide was established in Bemiparin sodium.The chromatographic conditions were determined as follows:the analysis is performed on Agilent ZORBAX Eclipse XDB-CN column(250×4.6 mm,5μm),the column temperature is set to 35℃,0.2 mol·L^(-1) sodium perchlorate solution(Adjusting pH vaule of 2.2 with 1 mol·L^(-1) perchloric acid)-acetonitrile(88∶12)is adopted as mobile phase,and the flow rate of 0.8 mL·min-1,the detection wavelength of 207 nm,and the sample volume of 50μL are adopted.The results show that the concentration of benzyltrimethylammonium hydroxide bears a good linear relationship with peak area within the range of 0.01 to 1.0μg·mL-1(r=0.9998,n=7);the RSD of the repeatability test results is 1.21%(n=6);the RSD of the intermediate precision test results is 1.35%(n=12);the RSD of the robustness test results is 1.20%(n=16);the stability of the solution is good within 48 hours with an RSD of 0.19%(n=13);the average recovery rate is 102.40%,with an RSD of 1.70%(n=9).This method is simple to operate,highly sensitive,and provides accurate and reliable results.It can be used for the determination of benzyltrimethylammonium hydroxide residues in Bemiparin sodium.
作者
邵昉
任风芝
刘建芬
王月
韩阳
李宁
Shao Fang;Ren Fengzhi;Liu Jianfen;Wang Yue;Han Yang;Li Ning(North China Pharmaceutical Group Corporation,New Drug Research and Development Corporation Ltd.,Shijiazhuang 052165,China;North China pharmaceutical Huakun Hebei Biotechnology Corporation Ltd.,Shijiazhuang 050000,China;Hebei Multi-component Biochemical Drug Preparation Technology Innovation Center,Shijiazhuang 050000,China)
出处
《煤炭与化工》
CAS
2024年第4期153-156,共4页
Coal and Chemical Industry
