HPLC法测定贝米肝素钠中苄基三甲基氢氧化铵的残留  

Resident determination of benzyltrimethylammonium hydroxide in bemiparin sodium by HPLC

作　　者：邵昉[1,3] 任风芝 刘建芬[2,3] 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)

机构地区：[1]华北制药集团新药研究开发有限责任公司,河北石家庄052165 [2]华北制药华坤河北生物技术有限公司,河北石家庄050000 [3]河北省多组分生化药物制备技术创新中心,河北石家庄050000

出　　处：《煤炭与化工》2024年第4期153-156,共4页Coal and Chemical Industry

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.

关 键 词：高效液相色谱法 贝米肝素钠 苄基三甲基氢氧化铵 残留 

分 类 号：O657.72[理学—分析化学]