摘要
目的建立反相高效液相色谱荧光法测定人血浆中巴洛沙星浓度。方法采用Diamonsil ODS C_(18)分析柱(200 mm×4.6 mm,5μm),柱温为室温,流动相为乙腈-0.05 mol·L^(-1)KH_2PO_4缓冲液(25:75,V/V)(三乙胺和H_3PO_4调pH为3.40),流速:1.0 mL·min^(-1);血浆样品用二氯甲烷旋涡混合后,提取有机层,在40℃条件下氮气吹干,残渣用流动相溶解进样,荧光检测器(λ_(cx)=295 nm,λ_(cm)500 nm)检测,以加替沙星作内标,按内标法定量。结果标准曲线在50～4 000μg·L^(-1)内线性良好,最低检测限为10μg·L^(-1),巴洛沙星及内标的保留时间分别为5.35和4.03 min,日内和日间RSD均<10.0%,提取回收率和方法回收率分别在92%～99%和95%～105%。结论本法具有快速、简便、灵敏、准确等优点,适用于人血浆中巴洛沙星浓度测定及药动学研究。
AIM To establish an RP-HPLC method with fluorescence detection for the determination of balofloxacin in human plasma. METHODS A fluorescence detector and Diamonsil ODS ClS analysis column （200 mm × 4.6 mm,5 μm） were used.The plasma sample was extracted with 4.0 mL dichloromethane.After evaporation of the organic layer, the residue was dissolved in 200 μL mobile phase and 20 μL was injected into the column. The mobile phase of acetonitril-0.05 mol· L^-1 potassium dihydrogen phosphate （25：75, V/V） was eluted at flow rate of 1.0 mol· L^-1 through the column. The detector at high sensitivity was set at λ ex 295 nm and λ ex 500 ran. RESULTS The retention time for balofloxacin and intemal standard （gatifloxacin） was 5.35 rain and 4.03 min, respectively. The standard curve was linear over the concentration range of 50 to 4 000 μg· L^- 1. The lowest concentration of detection in plasma was 10 μg· L^- 1 .The extraction recoveries and method recoveries were 92% - 99% and 95% - 105%, respectively. The intra-day RSD and inter-day RSD were less than 10%. CONCLUSION This method is simple, rapid, sensitive and accurate and suitable for clinical practical application.
出处
《中国临床药学杂志》
CAS
2007年第5期296-299,共4页
Chinese Journal of Clinical Pharmacy
