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目的建立人血浆中洛匹那韦的高效液相色谱测定方法,用于临床进行药物浓度监测。方法血浆样品经醋酸乙酯液液萃取后,采用高效液相色谱法(HPLC)进行分析。Eclipse C18柱分离,流动相采用甲醇-0.1 mol·L-1醋酸铵溶液,流速为1mL.min-1;梯度洗脱在0～6 min甲醇-0.1 mol·L-1醋酸铵溶液为70∶30,6.1～15 min甲醇-0.1 mol·L-1醋酸铵溶液为80∶20;利用光电二极管阵列检测器对流份进行双波长同时检测(洛匹那韦210 nm,内标298 nm),柱温30℃。结果内源性物质不干扰测定,洛匹那韦的线性范围为1～12 mg.L-1(r=0.997 0),最低定量限为1 mg.L-1,基质效应为92.11%～105.31%(n=5),萃取回收率为73.32%～89.50%(n=5),批内和批间精密度(RSD%)分别为1.75～5.99(n=5)和4.97～9.79(n=3)。结论建立的HPLC方法简便、灵敏、准确、所需样本量小,可以用于临床血药浓度测定。
Objective To establish a HPLC method for the determination of lopinavir in human plasma for the clinical monitoring of drug concentration. Methods Plasma samples were extracted with liquid ethyl acetate and analyzed by high performance liquid chromatography (HPLC). Eclipse C18 column, the mobile phase was methanol-0.1 mol·L-1 ammonium acetate solution, the flow rate was 1mL.min-1; gradient elution in 0 ~ 6 min methanol-0.1 mol·L-1 ammonium acetate solution was 70: 30, 6.1 ~ 15 min methanol-0.1 mol·L-1 ammonium acetate solution 80:20; using photodiode array detector for dual wavelength simultaneous detection (lopinavir 210 nm, internal standard 298 nm), column Temperature 30 ℃. Results The endogenous substances did not interfere with the determination. The linear range of lopinavir was 1 ~ 12 mg.L-1 (r = 0.997 0), the lowest limit of quantification was 1 mg.L-1, and the matrix effect was 92.11% -105.31 (n = 5), the recoveries were in the range of 73.32% -89.50% (n = 5). The intra- and inter-batch precision were 1.75 to 5.99 (n = 5) and 4.97 to 9.79 (n = 3). Conclusion The established HPLC method is simple, sensitive and accurate. The required sample size is small and can be used for the determination of clinical plasma concentration.