高效液相荧光色谱法测定人血浆中坎地沙坦的质量浓度

Content Determination of Candesartan in Human Plasma by HPLC-FLU

目的建立测定人血浆中坎地沙坦的高效液相荧光色谱法。方法血浆样品经20%高氯酸沉淀,色谱柱为BaiAn-C18柱(150 mm×4.6 mm,5μm),柱温为30℃,以甲醇-0.02 mmol/L磷酸盐缓冲液(pH=4.9,70∶30)为流动相,流速为1 mL/min,荧光检测激发波长(λex)为265 nm,发射波长(λem)为395 nm。结果血浆内源性杂质不干扰测定,坎地沙坦的质量浓度线性范围为2～300μg/L,定量下限为2μg/L,日内、日间精密度的RSD均小于8%。样品3次冻融、提取后,4℃下12 h内稳定性良好。结论该法灵敏、快速、准确,操作简便,可用于坎地沙坦的临床药代动力学研究。

Objective To establish an HPLC-FLU method for determination of candesartan in human plasma.Methods Plasma samples were treated by perchloric acid（20%）.Separation was carried out on the column of BaiAn-C18（150 mm×4.6 mm,5 μm） at 30 ℃.The mobile phase consisted of methanol-0.02 mmol/L potassium dihydrogen phosphate buffer（pH=4.9,70：30） pumped at a flow rate of 1 mL/min.The fluorescence detector was operated at an excitation and emission wavelengths of 265 nm and 395 nm,respectively.Results The intrinsic impurity of plasma did not interfere with the determination of analyte.The linear range of candesartan oxifen was 2-300 μg/L.Lower limit of quantification was 2 μg/L.The precision of inter-day and intra-day were less than 8%.The stability of unprocessed and processed samples stored at 4 ℃for 12 h was good.After 3 cycles of freeze and thaw processes,the plasma samples were stable.Conclusion The established HPLC-FLU method is fast,sensitive,and accurate and can be applied to the clinical pharmacokinetics investigations of candesartan.