Odou P, Robert H, Luyckx M, Brunet C, Dine T, Gressier B, Cazin M, Cazin J C
Department of Clinical Pharmacy, Faculty of Pharmaceutical and Biological Sciences, University Lille II, France.
Biomed Chromatogr. 1997 Jan-Feb;11(1):19-21. doi: 10.1002/(SICI)1099-0801(199701)11:1<19::AID-BMC611>3.0.CO;2-Z.
A routine high-performance liquid chromatographic method for measuring midazolam in human serum has been developed. The sample preparation procedure consisted of simple liquid-liquid extraction with dichloromethane, followed by evaporation under nitrogen. The mobile phase used was a mixture of acetonitrile at 0.02 M and sodium acetate at pH 3.0 (80:20, v/v) and a flow-rate of 1.2 mL/min. The separation was performed on two cyanopropyl columns (150 x 4.6 mm). The detection was by UV absorption at 240 nm. A linear range from 10 to 1,000 ng/mL and a quantification limit of 7.4 ng/mL of serum was reached. The mean intra-assay and inter-assay reproducibility from serum sample spiked with 100 ng/mL were 4.1 and 4.7%, respectively. The recoveries from serum sample spiked with 50, 100, 500 ng/mL were 85.46, 85.38 and 85.57%, respectively. This method was developed to allow pharmacokinetics study of midazolam in young patients in short surgical interventions.
已开发出一种用于测定人血清中咪达唑仑的常规高效液相色谱法。样品制备程序包括用二氯甲烷进行简单的液 - 液萃取，然后在氮气下蒸发。所用流动相为0.02 M乙腈和pH 3.0的醋酸钠的混合物（80:20，v/v），流速为1.2 mL/min。分离在两根氰丙基柱（150×4.6 mm）上进行。检测通过在240 nm处的紫外吸收进行。血清的线性范围为10至1000 ng/mL，定量限为7.4 ng/mL。加样浓度为100 ng/mL的血清样品的批内和批间平均重现性分别为4.1%和4.7%。加样浓度为50、100、500 ng/mL的血清样品的回收率分别为85.46%、85.38%和85.57%。开发该方法是为了能够对接受短期外科手术的年轻患者进行咪达唑仑的药代动力学研究。
