Qin Y, Zou Y, Yu Q, Liang M, Liu H, Rao G, Li Z, Li K
Institute of Clinical Pharmacology, Chengdu.
Hua Xi Yi Ke Da Xue Xue Bao. 1996 Mar;27(1):114-6.
This paper report a sensitive and rapid method for the determination of metronidazole (MTZ) using theophylline as the internal standard. High performance liquid chromatograph model 344 (Beckman) with a 254 nm wavelength UV detector and YWG-C18H37 column (10 microns, 250 x 4.6 mm) was used. To the serum sample 200 microliters, 100 microliters phosphate buffer (0.8 mol/L, pH 7.5) was added, then extracted with 3 ml chloroform containing 5% isopropyl alcohol. The organic layer was removed and evaporated to dryness under an air stream in a 40 degrees C water bath. The residue was dissolved in 30 microliters mobile phase and 20 microliters injected. The mobile phase of water-methanol (73:27) was pumped at 1.0 ml/min through the column. The detector operated at 0.005 aufs. The retention times for MTZ and theophylline were 5.78 and 6.81 min respectively. Standard curve was linear in the concentration range of 0.3125 to 20 mg/L. The detection limit in serum was 0.02 mg/L. Extraction recovery was 77%-82%; method recovery 99%-102%; withinday RSD less than 3.0%; inter-day RSD less than 3.5%.
本文报道了一种以茶碱为内标物测定甲硝唑（MTZ）的灵敏快速方法。使用配有254nm波长紫外检测器的344型高效液相色谱仪（贝克曼）和YWG-C18H37柱（10微米，250×4.6毫米）。向200微升血清样品中加入100微升磷酸盐缓冲液（0.8mol/L，pH7.5），然后用3毫升含5%异丙醇的氯仿萃取。除去有机层，在40℃水浴中于气流下蒸发至干。残渣溶于30微升流动相中并进样20微升。水-甲醇（73:27）流动相以1.0毫升/分钟的流速泵入柱中。检测器以0.005aufs运行。MTZ和茶碱的保留时间分别为5.78和6.81分钟。标准曲线在0.3125至20mg/L的浓度范围内呈线性。血清中的检测限为0.02mg/L。萃取回收率为77%-82%；方法回收率为99%-102%；日内相对标准偏差小于3.0%；日间相对标准偏差小于3.5%。
