摘要
目的建立一种简单、快捷、灵敏、准确的监测人血浆样品中维拉帕米的方法。方法采用SPE方法处理血浆样品;加洛帕米为内标,醋酸-醋酸钠溶液:甲醇:三乙胺(45:55:1)为流动相,应用HPLC色谱法配合荧光检测,荧光检测波长275nm。结果所得色谱图中维拉帕米与内标能很好分离,无明显杂质峰的影响。建立的方法经验证,线性范围为5~500ng.mL-1,检测限为1.4ng.mL-1,定量限为5.0ng.mL-1,平均加样回收率分别是90.7%、88.2%和90.2%,精密度试验RSD值<15%,各种稳定性试验中RSD值均<20%。结论该方法简单、快捷、灵敏、准确,适用于临床维拉帕米的血药浓度监测。
Objective To develop a simple,fast,sensitive,accurate method to monitor verapamil in human plasma samples. Methods To employ a SPE approach for plasma samples treatment;Gallo verapamil as internal standard, acetic acid-sodium acetate:methanol:triethylamine(45 : 55 : 1)as mobile phase,to detect by HPLC chromatography with fluorescence,fluorescence detection wavelength 275 nm. Results The peaks of verapamil and internal standard in the chromatograms can be well separated,no obvious peak of the impurity can be observed.The method have been validated and the linear range was 5 - 500 ng·mL-1,limit of detection was 1.4 ng·mL-1,limit of quantification was 5.0 ng·mL-1,the average recoveries were 90.7%,88.2% and 90.2%,and the value of RSD of the precision was less than 15%,the RSD value in the stability test are less than 20%. Conclusion The method is simple,fast, sensitive and accurate and can applicable to blood concentration monitoring of verapamil in clinical.
出处
《中国医药科学》
2012年第13期97-98,共2页
China Medicine And Pharmacy
基金
广东省中医药管理局课题(20112028)