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目的优化头孢氨苄血药浓度测定方法。方法采用HPLC法,以头孢哌酮为内标,YWGC18色谱柱(4.6 mm×250 mm,10μm),以水-甲醇-2.5 mol.L-1醋酸铵-冰醋酸(体积比为90.000∶30.000∶0.450∶0.016)为流动相,流速为1.0 mL.min-1,检测波长为254 nm;柱温为室温。结果血浆样品的预处理:精密吸取全血分离血浆0.5 mL于具塞塑料离心管中,加入0.1 mL头孢哌酮(100 mg.L-1内标)和0.2 mL的质量分数为10%的三氯乙酸沉淀试剂,漩涡震荡1 min混合后10 000 r.min-1离心5 min,取上清液进样测定。以头孢氨苄峰面积和内标峰面积比(Y)对头孢氨苄浓度(X)回归分析,方程为Y=0.121 5X+0.032 1,r=0.999 5(n=7),线性范围为0.5～100.0 mg.L-1,提取回收率>88.83%(n=5),方法回收率为92.6～102.6%,日内RSD≤3.46,日间RSD≤5.71%,且稳定性良好。结论HPLC法可用于测定头孢氨苄的血药浓度。
Objective To optimize the determination of cephalexin serum concentration. Methods HPLC was performed on a YWGC18 column (4.6 mm × 250 mm, 10 μm) using water with methanol-2.5 mol·L-1 ammonium acetate-glacial acetic acid (volume ratio 90.000:30.000: 0.450:0.016) as the mobile phase at a flow rate of 1.0 mL · min-1 with a detection wavelength at 254 nm. The column temperature was at room temperature. Results Pretreatment of plasma samples: Precision draw whole blood 0.5 mL plasma was centrifuged in a plastic tube, add 0.1 mL cefoperazone (100 mg.L-1 internal standard) and 0.2 mL of 10% by mass of tris Chloroacetate precipitation reagent, vortex vortex 1 min after mixing 10 000 r.min-1 centrifugation 5 min, the supernatant was injected. The regression equation of the concentration of cephalexin (X) with the area ratio of cephalexin and the peak area of the internal standard (Y) was obtained. The equation was Y = 0.121 5X + 0.032 1, r = 0.999 5 (n = 7) with a linear range of 0.5-100.0 The recovery rate was 92.6% ~ 102.6%. The RSD≤3.46, RSD≤5.71%, and the stability was good. Conclusion HPLC method can be used to determine the plasma concentration of cephalexin.