Zeng J, Liu D, Zou Y
Hua Xi Yi Ke Da Xue Xue Bao. 1992 Sep;23(3):321-4.
A high-performance liquid chromatographic method for the determination of p-hydroxyphenytoin (p-HDPH) in human urine was reported. Following acid hydrolysis of urine sample at 90 degrees C for 1 h, an internal standard, nitrophenol, was added. The sample was extracted with n-hexane-ethyl acetate (50:50), and organic layer was evaporated. The residue was dissolved in methanol and chromatographed on an Ultrasphere-ODS column, using a mobile phase of phosphate buffer (0.03 mol/L, pH 6.0): methanol (65:35) at a flow rate of 0.8 ml/min. The eluent was monitored at 240 nm. The standard curve was linear within the range 5.0-200 micrograms/ml (r = 0.9998). Analytical recovery rates were 102.8 +/- 7.3% (p-HDPH 9.70 micrograms/ml, n = 5) and 104.9 +/- 6.4% (p-HDPH 54.70 micrograms/ml, n = 5). The cumulative recovery of p-HDPH in 0-12 h volunteers' urine samples accounted for 20% of the oral dose of 100 mg phenytoin sodium.
报道了一种测定人尿中对羟基苯妥英（p-HDPH）的高效液相色谱法。尿样在90℃酸水解1小时后，加入内标物硝基苯酚。样品用正己烷 - 乙酸乙酯（50:50）萃取，有机层蒸发。残渣溶于甲醇，在Ultrasphere-ODS柱上进行色谱分析，流动相为磷酸盐缓冲液（0.03 mol/L，pH 6.0）：甲醇（65:35），流速为0.8 ml/min。在240 nm处监测洗脱液。标准曲线在5.0 - 200微克/毫升范围内呈线性（r = 0.9998）。分析回收率为102.8±7.3%（p-HDPH 9.70微克/毫升，n = 5）和104.9±6.4%（p-HDPH 54.70微克/毫升，n = 5）。0 - 12小时志愿者尿样中p-HDPH的累积回收率占口服100毫克苯妥英钠剂量的20%。
