Liu G L, Sha R G, Gao S, Shen Y X, Wang S X
Department of Clinical Pharmacology, Changhai Hospital, Second Military Medical University, Shanghai.
Yao Xue Xue Bao. 1993;28(3):216-21.
A double column and double pump HPLC switching system is described for the analysis of cefixime in human plasma and urine. The system used muBondapak C18 short pretreatment column for on-line sample clean-up and a Hitachi GEL 3056 (ODS) analytical column for separation. A mixed solution of 0.01 mol/L H3PO4-0.1 mol/L KH2PO4-H2O (20:1:79) was used as the pretreatment mobile phase and CH2CH-0.01 mol/L H3PO4-0.1 mol/L KH2PO4-H2O (13:20:1:66) was used as analytical mobile phase. The compound in plasma and urine is detected by ultraviolet absorption at 286 nm and 314 nm, respectively. The absolute recoveries of the method in plasma and urine were 99.1% and 98.6% respectively. The relative standard deviations of the method are 0.70-3.82% and 0.80-3.73% in plasma, 1.53-3.08% and 1.31-2.67% in urine between days and day-to-day. Linear calibration curve for cefixime was measured over the range of 0.1-3.2 micrograms/ml in plasma and 1.0-32.0 micrograms/ml in urine, and the correlation coefficients were all 0.9999. The detection limit was 0.05 micrograms/ml in plasma and 0.2 micrograms/ml in urine. The plasma and urine samples were diluted with water and injected directly onto the HPLC system. The operation is simple and the relative sensitivity is markedly increased because of higher recoveries and larger loading capacity of the sample.
描述了一种用于分析人血浆和尿液中头孢克肟的双柱双泵高效液相色谱切换系统。该系统使用μBondapak C18短预处理柱进行在线样品净化,并使用日立GEL 3056(ODS)分析柱进行分离。0.01 mol/L H3PO4 - 0.1 mol/L KH2PO4 - H2O(20:1:79)的混合溶液用作预处理流动相,CH2CH - 0.01 mol/L H3PO4 - 0.1 mol/L KH2PO4 - H2O(13:20:1:66)用作分析流动相。血浆和尿液中的化合物分别通过286 nm和314 nm处的紫外吸收进行检测。该方法在血浆和尿液中的绝对回收率分别为99.1%和98.6%。该方法在血浆中日内和日间的相对标准偏差分别为0.70 - 3.82%和0.80 - 3.73%,在尿液中分别为1.53 - 3.08%和1.31 - 2.67%。头孢克肟的线性校准曲线在血浆中为0.1 - 3.2微克/毫升,在尿液中为1.0 - 32.0微克/毫升范围内测定,相关系数均为0.9999。血浆中的检测限为0.05微克/毫升,尿液中的检测限为0.2微克/毫升。血浆和尿液样品用水稀释后直接注入高效液相色谱系统。该操作简单,并且由于回收率较高和样品负载量较大,相对灵敏度显著提高。