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目的建立一种快速简便的高效液相色谱法测定人血浆中非索非那定的浓度,以适合于大样本的血浆样品测定需要。方法以乙腈沉淀法处理200 L血浆样品,高速离心后上清液用纯氮气吹干,复溶后进样分析。分析柱:WatersSymmetry C18色谱柱(4.6 mm×250 mm,5 m);流动相:0.1 mol.L 1醋酸铵溶液-乙腈(63∶37);流速:1 mL.min 1;荧光检测器(激发波长为230 nm,发射波长为290 nm);以苯海拉明为内标,用内标法定量,进行方法学确证试验,并用于4名健康志愿者单剂量口服120 mg非索非那定片剂的药动学研究。结果内源性杂质和代谢物不干扰非索非那定出峰。在20~1 000 g.L1内线性良好(r=0.999 3,n=6),定量限为20 g.L1。高、中、低质控样品的日内、日间RSD均<10%,方法学回收率为105.9%,提取回收率为94.6%。平均Cmax,tmax和AUC0~t分别为733 g.L1,2.5 h和3 954 g.h.L1,这些参数与国外文献报道基本一致。结论本测定方法稳定、操作简便、快速、准确、灵敏,可用于非索非那定药动学研究。
OBJECTIVE: To establish a rapid and simple HPLC method for the determination of fexofenadine in human plasma, which is suitable for the determination of plasma samples in large samples. Methods 200 L plasma samples were treated with acetonitrile precipitation method. After high speed centrifugation, the supernatant was dried with pure nitrogen and injected into solution for analysis. Analytical column: Waters Symmetry C18 column (4.6 mm × 250 mm, 5 m); mobile phase: 0.1 mol·L 1 ammonium acetate solution-acetonitrile (63:37); flow rate: 1 mL.min 1; Wavelength of 230 nm, emission wavelength of 290 nm); diphenhydramine as internal standard, internal standard method for confirmatory tests, and for four healthy volunteers single dose oral 120 fexofenadine Pharmacokinetic study of tablets. Results Endogenous impurities and metabolites did not interfere with fexofenadine peak. The linearity was good (r = 0.999 3, n = 6) in 20-1 000 g.L1 and the limit of quantification was 20 g.L1. RSDs of day, day and day for high, medium and low quality control samples were all less than 10%, the methodological recovery rate was 105.9% and the extraction recovery rate was 94.6%. The average Cmax, tmax and AUC0 ~ t were 733 g.L1, 2.5 h and 3 954 g.h.L1, respectively, and these parameters were basically consistent with those reported in foreign literature. Conclusion The method is stable, simple, rapid, accurate and sensitive. It can be used in the study of felodipine pharmacokinetics.