高效液相色谱法测定盐酸普萘洛尔中同分异构体杂质β-普萘洛尔的含量
Determination of isomeric impurity β-propranolol content in propranolol hydrochloride by HPLC
崔萍 1商少华 1曹庆丰1
作者信息
- 1. 江苏省药物研究所药品检测及包材相容性研究中心,江苏省药物研究所有限公司,南京 211816
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摘要
目的 建立HPLC法测定盐酸普萘洛尔中同分异构体杂质β-普萘洛尔的含量.方法 采用YMC-PackODS-AQ(150 mm×4.6 mm,3 μm)色谱柱,以十二烷基硫酸钠和磷酸二氢四丁基铵溶液-乙腈(70∶30)为流动相A,以十二烷基硫酸钠和磷酸二氢四丁基铵溶液-乙腈(30∶70)为流动相B,在线等度洗脱A-B(70∶30),流速为0.8mL·min-1,检测波长为225 nm,进样体积为20 μL.结果 β-普萘洛尔检测限为0.1 ng,定量限为0.3 ng;β-普萘洛尔在0.015～1.981 μg·mL-1内呈良好的线性关系(r=0.9999);低、中、高水平的平均回收率分别为 99.06％、100.4％、100.5％,RSD分别为 0.18％、0.10％、0.060％(n=3).结论 本法简便、灵敏、准确、可靠,可为盐酸普萘洛尔原料药中β-普萘洛尔的质量控制提供参考.
Abstract
Objective To determine the content of isomeric impurity β-propranolol in propranolol hydrochloride by HPLC.Methods YMC-Pack ODS-AQ(150 mm × 4.6 mm,3 μm)chromatographic column was used.Mobile phase A was lauryl sodium sulfate and four butyl ammonium dihydrogen phosphate solution-acetonitrile(70∶30),while mobile phase B was lauryl sodium sulfate and four butyl ammonium dihydrogen phosphate solution-acetonitrile(30∶70).The online isocratic elution A-B(70∶30)was used,the flow rate was 0.8 mL·min-1,the detection wavelength was 225 nm,and the injection volume was 20 μL.Results The limit of detection of β-propranolol was 0.1 ng and the limit of quantification was 0.3 ng;β-propranolol showed good linearity within 0.015～1.981 μg·mL-1(r=0.9999);the average recovery at low,medium,and high concentration levels was 99.06％,100.4％,and 100.5％,while the RSD was 0.18％,0.10％,and 0.060％(n=3).Conclusion This method is simple,sensitive,acurate and reliable,which provides reference for the quality control of β-propranolol in propranolol hydrochloride.
关键词
盐酸普萘洛尔/同分异构体杂质/β-普萘洛尔/HPLC法Key words
propranolol hydrochloride/isomeric impurity/β-propranolol/HPLC引用本文复制引用
出版年
2024
NETL
NSTL
万方数据