摘要
目的建立测定血浆中伊伐布雷定浓度的高效液相-荧光（FLU）测定方法，用于临床血浆伊伐布雷定浓度的测定。方法血浆样品经VarianC2柱固相萃取后采用HPLC-FLU法在Kromasil@C18柱分离，流动相采用乙腈-10mmol·L^-1磷酸二氢钾（含0．3％10mmol·L^-1盐酸）（28：72），流速为1mL·min^-1，柱温为25℃，荧光检测波长：λ1=328nm，λ2=283nm。结果内源性杂质不干扰测定，伊伐布雷定在0．5—50μg·L^-1内线性良好（r=0．9996），最低定量限为0．5μg·L^-1。萃取回收率为78．74％～90．77％（n=5），批内和批问精密度（RSD％）分别为2．53～6．33（n=6）和6．38～8．91（n=3）。结论建立的固相萃取-HPLC—FLU方法简便、灵敏、准确、所需血浆量少，可以用于临床血药浓度测定。
OBJECTIVE To develop a HPLC-FLU method for the determination of ivabradine in plasma. METHODS The plasma samples with Varian C2 solid-extraction pretreatment were separated on a Kromasil C18 column, using acetonitrile-10 mmol ·L^-1 KH2PO4 （containing 0. 3% 10 mol · L^-1 hydroehloride） （28： 72） as the mobile phase. The flow rate was 1.0 mL · min^-1 at room temperature. Detection was carried out at hi = 328 nm and k2 = 283 rim. RESULTS The method was linear for ivabradine in the range of 0. 5 - 50 μg · L ^- 1. The correlation coefficient was 0. 999 6 and the LLOQ was 0. 5 μg · L ^- 1. The extraction recoveries were in the range of 78.74% - 90. 77% （ n = 5 ）. The intra-day and inter-day precisions （ RSD% ） were 2, 53 - 6. 33 （ n = 6） and 6. 38 - 8. 91 （ n = 3）. CONCLUSION The HPLC-FLU method was simple, sensitive and accurate. It was suitable for the determination of ivabradine in plasma.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2010年第4期307-310,共4页
Chinese Pharmaceutical Journal
基金
科技部"国家科技重大新药创制"专项资助(2008ZX09312-010)
关键词
伊伐布雷定
荧光
固相萃取
血浆
ivabradine
fluorescence detection
solid-extraction
plasma
