摘要
为了建立一种盐酸阿考替胺原料药含量的测定方法,采用高效液相色谱法(HPLC),使用Agilent ZORBAX SB-C18色谱柱(25 cm×4.6 mm,5μm);柱温:30℃;检测波长:230nm;流速:1.0 m L/min;进样量:20μL;流动相:缓冲液(0.02 mol/L磷酸氢二钠加0.1%三乙胺溶液,稀磷酸调节pH值至3.0)∶乙腈=65∶35;稀释剂:流动相。结果表明,专属性研究结果显示盐酸阿考替胺保留时间为5.45 min,运行平稳,无杂质干扰;盐酸阿考替胺在0.20~0.60 mg/m L的浓度下,线性方程y=58.947x-0.201 7 (r2=0.999 7),线性关系良好;检测限为0.121μg/mL,定量限为0.452μg/mL;溶液稳定性试验证明供试品溶液24 h内稳定性较好,RSD为0.23 (n=7);重复性与中间精密度试验结果的RSD分别为0.10%(n=6)与0.14(n=12),重复性与中间精密度良好;耐用性考察的试验结果相对保留时间的RSD为1.05%(n=9),含量测定的RSD为0.13%(n=9);3批自制样品含量测定结果分别为99.11%、99.16%、99.09%。该方法数据准确可靠、检测快速、灵敏度高、耐用性强,可用于测定盐酸阿考替胺原料药的含量。
In order to develop a method for the determination of the content of acetamide in hydrochloride.The High-performance liquid chromatography(HPLC)was used with an Agilent ZORBAX SB-C18 column(25 cm×4.6 mm,5μm)as the analytical column;column temperature:30℃;detection wavelength:230 nm;flow rate:1.0 mL/min;injection volume:20μL;mobile phase:buffer solution(0.02 mol/L sodium dihydrogen phosphate solution with 0.1%triethanolamine,diluted with dilute phosphoric acid to pH=3.0):acetonitrile=65∶35;diluent:mobile phase.Results show that acotiamide hydrochloride had a retention time of 5.45 min,ran smoothly,and there was no interference from impurities.Acotiamide Hydrochloride had a good linear relationship with a linear equation of y=58.947x-0.2017(r2=0.9997)at a concentration of 0.20~0.60 mg/mL.The detection limit was 0.121μg/mL,the quantitative limit was 0.452μg/mL;the stability test of the sample solution showed that the stability was good within 24 h,with an RSD of 0.23(n=7);the RSDs of repeatability and intermediate precision were 0.10%(n=6)and 0.14(n=12),respectively,indicating good repeatability and intermediate precision;the RSD of the durability test was 1.05%(n=9),and the RSD of the content determination was 0.13%(n=9);the content determination results of three self-prepared samples were 99.11%,99.16%,and 99.09%.
作者
董永广
Dong Yongguang(Hebei Jiheng Pharmaceutical Corporation Ltd.,Hengshui 053400,China)
出处
《煤炭与化工》
2025年第6期152-156,共5页
Coal and Chemical Industry
关键词
高效液相色谱法
盐酸阿考替胺
含量测定
high performance liquid chromatography
acotiamide hydrochloride trihydrate
content
