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目的建立人血浆水飞蓟宾检测的高效液相色谱方法。方法以卡马西平为内标,在酸性条件下,血浆经乙酸乙酯和正己烷萃取,以ZORBAX Eclipse XDB-C18为分析柱,流动相为乙腈-水-0.1%三氟乙酸(34∶36∶30),流速为0.8 mL.min-1;检测波长288 nm。结果水飞蓟宾浓度在0.05～6.00 mg.L-1内线性关系良好(r=0.9997);低、中、高3种浓度(0.1,1.0,4.0 mg.L-1)的相对回收率分别为(99.2±4.9)%,(101.8±3.5)%和(100.7±2.6)%;日内精密度RSD分别为3.8%,2.7%和2.2%,日间精密度RSD分别为4.9%,3.3%和2.0%。结论该方法准确可靠、简便快速,适用于人血浆水飞蓟宾的测定及其药代动力学研究。
Objective To establish a high performance liquid chromatographic method for the determination of silybin in human plasma. Methods Carbamazepine was used as an internal standard. Under acidic conditions, the plasma was extracted with ethyl acetate and n-hexane. The mobile phase was ZORBAX Eclipse XDB-C18 with acetonitrile-water-0.1% trifluoroacetic acid (34:36 : 30) at a flow rate of 0.8 mL.min-1 and a detection wavelength of 288 nm. Results The linear range of silybin was 0.05 ~ 6.00 mg.L-1 (r = 0.9997). The relative recoveries of low, medium and high concentrations (0.1, 1.0 and 4.0 mg.L-1) Were (99.2 ± 4.9)%, (101.8 ± 3.5)% and (100.7 ± 2.6)%, respectively. The intra-day precision RSD was 3.8%, 2.7% and 2.2% respectively. The intraday RSD was 4.9%, 3.3% and 2.0%. Conclusion The method is accurate, reliable, simple and rapid, suitable for the determination of silybin in human plasma and its pharmacokinetics.