RP-HPLC-FLD法测定盐酸氟桂利嗪片中盐酸氟桂利嗪的含量及含量均匀度

Determination of Flunarizine Hydrochloride and Content Uniformity Test in Flunarizine Hydrochloride Tablet by RP-HPLC-FLD

目的：运用反相高效液相色谱联合荧光检测器法测定盐酸氟桂利嗪片中盐酸氟桂利嗪的含量及含量均匀度。方法：采用DiamonsilTMC18柱（250mm×4.6mm，5耻m）．以甲醇：0．02mol／L磷酸二氢铵（0．1％三乙胺，磷酸调pHi3．0）（70：30）为流动相．流速为ImL／min，激发波长260nm．发射波长310nm，柱温为25℃，进样体积10μL，进行了方法学考察和盐酸氟桂利嗪的含量及均匀度测定。结果：盐酸氟桂利嗪在6．1～122ng（r=0．9992）范围内呈良好的线性关系．平均回收率为100．07％（RSD=1．38％）：LOD（1imit of detection）和LOQ（1imit of quantification）分别为2．44ng、8．13ng；盐酸氟桂利嗪片三批样品的平均标示量分别为98．27％、98．79％、99．89％，其含量均匀度A＋I．8S分别为5．644、4．194、7．160，均小于15。结论：该方法快速、准确，无杂质干扰．可为盐酸氟桂利嗪片的质量标准的建立与完善提供科学依据并指导临床合王早用药．

Objective： To develop a method to determine tbe content of flunarizine hydrochloride in flunarizine hydrochloride content by RP - HPLC-fluorescence detector and test the content uniformity. Methods： DiamonsilTM C18 column （250mm × 4.6mm, 5μm） was used, with 70：30 methanol and 0.02mol/L ammonium dihydrogenphosphate （0.1% triethylamine, pH adjusted to 3.0 by phosphoric acid） as mobile phase. The flow rate was lmL/min. Excitation wavelength was 260rim, and the emission wavelength was 310nm. The column temperature was 25℃ with sample volume at 10μl. Remalts： The Standard curve of flunarizine hydrochloride had good linear relationship within 6.1-122ng （t-=0.9992）.The average recovery was 100,07% （RSD=1.38%）. Limit of detection and limit of quantification were 2.44ng and 8.13ng, respectively. The average percentage of actual content to marked quantity of the three batch samples were 98.27%, 98.79%, 99.89% respectively. Content uniformity A＋I.8S were 5.644, 4.194, and 7.160 respectively, all below 15. Conclusion： The method was rapid and accurate, with nointerference from internal components of flunarizine hydrochloride tablets, which provided a scientific basis for quality standard establishment and clinical rational drug use.