HPLC-CAD法测定盐酸乙胺丁醇片中盐酸乙胺丁醇的含量

目的建立高效液相-电雾检测器（HPLGCAD）方法测定盐酸乙胺丁醇片剂中盐酸乙胺丁醇（EMB）的含量。方法采用安捷伦1200系列高效液相色谱系统联合电雾式检测器测定。流动相溶解片剂样品，涡旋约30min，过滤后注入色谱系统。色谱柱为HederaODS-2C18柱（250mm×4．6mm，5μm），柱温：40℃，流动相：15mm01·L^-1醋酸铵溶液（pH7．3）-甲醇（80：20，v／v），流速：1．0mL·min^-1，进样体积：20μL。CAD参数：气压35psi（housenitrogen），量程100pA。结果此方法测定EMB的最低定量限（LOQ）为15μg·mL^-1（S／N=10），方法回收率〉99．84％，日间、日内精密度均〈3．50％，线性范围为25-200μg·mL^-1（r〉0．9999）。片剂的赋形剂对EMB的含量测定几乎没有干扰。结论本方法准确、快速、简便，可用于EMB的测定及其释放度和稳定性研究，对其类似化合物的测定具有参考价值。

Determination of ethambutol hydrochloride in tablets by high performance liquid chromatography with charge aerosol detection (HPLC-CAD)

Objective To establish a high performance liquid chromatographic with charge aerosol detection （HPLCCAD） method for the determination of ethambutol hydrochloride （EMB） in tablets. Methods An Agilent 1200 Series HPLC system with a charged aerosol detector was used. The tablet samples were dissolved by mobile phase, broken down by vortex mixing apparatus for approximately 30 min. The samples were injected into a Hedera ODS-2 C18 （250 mm×4.6 ram, 5μm） column at 40℃. The mobile phase was composed of 15 mmol·L^-1 ammonium acetate （pH 7.3） - methanol （80 ： 20, v/v）, with a flow rate of 1.0 mL·min^-1. The injection volume was 20 μL. The CAD parameters were： gas 35 psi （house nitrogen）, and range 100 pA. Results The limit of quantitation （LOQ） was 15μg·mL ^-1（S/N= 10）. The methodology recovery was higher than 99.84：%. The intra-day and inter-day RSD were less than 3.50%. The calibration curve was linear at 254200μg·mL^-1, with coefficient of determination over 0. 999 9. EMB was detected with little interference from the excipient blend of the tablets. Conclusion The method is accurate, rapid and convenient for release and stability test of EMB and may be used as reference for similar compounds.