摘要
目的:建立测定痕量瑞格列奈的方法,并用于瑞格列奈片的溶出度研究。方法:采用高效液相色谱-荧光检测法。色谱柱为C18,流动相为0.5%磷酸(pH调至2.5)-甲醇-乙腈(40∶10∶50),流速为1.0mL·min-1,柱温为40℃,进样量为20μL,荧光检测波长为λex=244nm、λem=348nm。溶出度测定方法为桨法,溶出介质为枸橼酸-磷酸盐缓冲液(pH=5.0),转速为75r·min-1,测定3批片剂在60min内的累积溶出度。结果:瑞格列奈检测浓度线性范围为0.055～1.76μg·mL-1(r=0.9997),低、中、高浓度平均回收率分别为98.8%、99.4%、99.6%(RSD=1.4%、1.3%、1.5%),最低定量限0.21ng,最低检测限0.05ng。3批片剂30min时累积溶出度为89.6%～93.4%。结论:该方法灵敏度高、专属性强,适用于瑞格列奈的痕量测定及满足大杯法研究瑞格列奈片的溶出度的要求。
OBJECTIVE： To establish the method for the trace determination and dissolution study of Repaglinide tablets. METH- ODS： HPLC-fluorescence detection was adopted. A separation was performed on Kromasil C18 column, the mobile phase was 0.5% phosphonic acid （pH adjusted to 2.5）-methanol-acetonitrile （40 ： 10 ： 50） with the flow rate at 1.0 mL. min 1. The column temperature was 40 ℃and injection volume 20 μL. The wavelengths of excitation and emission were set at 244 nm and 348 nm, respectively. The dissolution of Repaglinide tablets was detected by paddle method using citric acid-phosphate buffer solution （pH= 5.0） as solvent at rotation speed of 75 r. min^-1. The accumulative dissolution of 3 batches of samples was determined. RESULTS： The linear range of repaglinide was 0.055~1.76 μg.mL^-1 （r=0.999 7） with average recoveries of 98.8%, 99.4% and 99.6% at low, medium and high concentration （RSD= 1.4%, 1.3%, 1.5% ）. The quantitative limit was 0.21 ng and detection limit was 0.05 ng. The accumulative dissolution of 3 batches of samples at 30 min was 89.6 % ~93.4 %. CONCLUSION： The method is sensitive and specific for the trace determination and dissolution of repaglinide.
出处
《中国药房》
CAS
CSCD
北大核心
2011年第9期841-843,共3页
China Pharmacy
