North China Pharmaceutical Group Corporation, New Drug Research and Development Corporation Ltd.
North China pharmaceutical Huakun Hebei Biotechnology Corporation Ltd. ,Shijiazhuang 050000, China
Hebei Multi-component Biochemical Drug Preparation Technology Innovation Center

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，5 μm），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50 μL。结果表明，苄基三甲基氢氧化铵质量浓度在 0. 01～1.0 μg/mL范围内与峰面积线性关系良好（r =0. 999 8，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,5 μm）, 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 50 μL 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 1.0 μg·mL-1 (r=0.999 8, 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.

邵 昉1,3，任风芝1,3，刘建芬2,3，王 月1,3，韩 阳1,3，李 宁1,3. HPLC法测定贝米肝素钠中苄基三甲基氢氧化铵的残留[J]. 煤炭与化工, 2024, 47(4): 153-156.

Shao Fang1,3, Ren Fengzhi1,3, Liu Jianfen2,3, Wang Yue1,3, Han Yang1,3, Li Ning1,3. Resident determination of benzyltrimethylammonium hydroxide in bemiparin sodium by HPLC. CCI, 2024, 47(4): 153-156.