高效液相色谱法测定大鼠血浆和肺泡灌洗液中环丙沙星浓度  

HPLC method for the determination of ciprofloxacin concentration in rat plasma and bronchoalveolar lavage fluid

作　　者：梅和坤[1] 王瑾[1] 柴栋[2] 王睿[1] 夏蕾[3] 倪文涛[4] 

机构地区：[1]解放军总医院药物临床研究中心,北京100853 [2]解放军总医院临床药学中心,北京100853 [3]解放军总医院药学部,北京100853 [4]解放军总医院呼吸科,北京100853

出　　处：《中国临床药理学杂志》2017年第9期817-820,共4页The Chinese Journal of Clinical Pharmacology

基　　金：国家"十二.五"重大科技专项基金资助项目(2012ZX0903004-002)

摘　　要：目的建立一种测定大鼠血浆和肺泡灌洗液中环丙沙星浓度的高效液相色谱(HPLC)法。方法用甲醇直接蛋白沉淀法、去离子水直接稀释法分别对血浆和肺泡灌洗液进行处理,离心取上清,以莫西沙星为内标,用HPLC测定。色谱柱:Agilent SB-C18柱(4.6 mm×150 mm,5μm),流动相:乙腈-0.1%甲酸水,流速:1.0 m L·min^(-1),柱温:25℃,进样量:15μL。考察该方法的专属性、标准曲线与最低定量下限、精密度与回收率、稳定性。结果血浆和肺泡灌洗液中的内源性物质不影响环丙沙星的测定。在血浆和肺泡灌洗液中,环丙沙星分别在1.00~100.00μg·m L^(-1)(r=0.999 6)、0.05~2.00μg·m L^(-1)(r=0.998 5)内线性关系良好,最低定量下限分别为1.00和0.05μg·m L^(-1)。环丙沙星在血浆和肺泡灌洗液中的批内精密度分别为0.49%~3.77%和2.21%~5.00%,批间精密度分别为7.72%~8.83%和6.84%~9.51%,提取回收率分别为104.61%~113.29%和100.65%~103.96%;环丙沙星血浆和肺泡灌洗液稳定性符合相关要求。结论该方法简单、准确、可操作性强,适用于伏立康唑大鼠血浆及肺泡灌洗液浓度测定。Objective To establish a sensitive and reliable HPLC method for the determination of ciprofloxacin in rat plasma and bronchoalveolar lavage fluid （BALF）, ,and to apply this method for Pharmacokinetics, Methods Plasma sample and BALF sample were precipitated by methanol and dilution with water respectively, moxifloxacin was used as internal standard, the analytes were separated on an Agilent SB -C18 column （4. 6 mm× 150 mm,5μm）using the mobile phase of acetonitrile and 0. 1% formic acid in water at a flow rate of 1.0 mL · min^- 1, column temperature was 25 ℃. Results Chromatograms Showed no endogenous interfering peaks in the respective blank human plasma and BALF samples. The calibration curves for plasma and BALF were linear over a wide concentration range of 1.O0- 100.O0μg · mL-l（ r = O. 999 6）and O. 05 - 2.O0 μg · mL^-1 （ r = 0. 998 5 ） with a lower limit of quantification ofl μg · mL^-1 and 0.05 μg · mL^-1.The Inter-day and intra-day RSD of plasma and BALF were 0. 49% - 3.77%, 2.21% - 5.00% , 7.72% -8.83%, 6.84% - 9.51% , respectively. The extraction recovery of plasma and BALF were 104.61% - 113.29% and 100. 65% - 103.96%. Data of stability study fitted the request. accurate for the determination of ciprofloxacin in human plasma pharmacokinetic study of ciprofloxacin. Conclusion The method is simple, sensitive and and BALF samples. It could be widely used for pharmacokinetic study of ciprofloxacin.

关 键 词：高效液相色谱 环丙沙星 血药浓度 肺泡灌洗液 

分 类 号：R978.1[医药卫生—药品]