摘要
目的建立柱切换技术和限进性填料柱-HPLC法,实现在线直接进样并检测大鼠血浆中的呋塞米含量。方法以自制限进填料柱为预处理柱,Luna C18柱为分析柱,预处理流动相为水-甲醇(95:5,V/VA),含体积百分数为0.1%的甲酸,分析流动相为甲醇-水(65:35,V/V),流速均为1ml·min-1,柱温为25℃;检测波长为274nm。结果呋塞米血浆样品在进样100m时,富集效果良好,在0.1~3.2Ixg·ml-1的浓度范围内具有良好的线性关系(r=0.9995),高、中、低(0.4、0.8、1.61μg·ml-1)3个浓度血样的平均回收率分别为111.31%、104.48%和99.76%,日内日间精密度均小于5%。结论本方法简单快速,适用于血浆中呋塞米的直接进样检测。
Objective To establish a method of restricted-access media combined with HPLC in order to achieveonline direct injection and detection of furosemide in rat plasma. Methods The column of restricted access media was used as a pre-treatment column and a Cls column as the analytical column. The mobile phase of the pre- treatment column was water-methanol(95: 5, V/V ) and that of the analytical column was methanol-water(65:35, V/V ) at a flow rate of 1 ml "min-1. The wavelength was set at 274 nm and the column temperature at 25 ℃. Re- suits The calibration curve showed an excellent linear relationship ( r = 0. 9995 ) in the concentration range of 0.1 to 3.2 μg ·ml- 1 for furosemide in rat plasma. The average recovery of furosemide at 3 spiked levels was 111.31%, 104.48% and 99.76% respectively for plasma. The intra-day and inter-day assay precision and accuracy were good and the relative standard deviations (RSDs) were less than 5%. Conclusion This method for detection of furose- mide in plasma using restricted-access media-HPLC is simple and quick.
出处
《解放军药学学报》
CAS
2014年第3期200-203,共4页
Pharmaceutical Journal of Chinese People's Liberation Army
基金
国家科技部重大资助项目
No.2008ZXJ09014-010
全军医药科研"十二五"重点项目
No.BWS12J012
全军医药科研"十二五"面上项目
No.CWS11C231