Yuan Yue, Chen Xiaoyan, Zhong Dafang
School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenyang 110016, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Jun 1;852(1-2):650-4. doi: 10.1016/j.jchromb.2007.01.036. Epub 2007 Feb 1.
A highly sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS-MS) method was developed to determine meloxicam of low concentration in human plasma. After a simple sample preparation procedure by one-step protein precipitation with methanol, meloxicam and the internal standard piroxicam were chromatographed on a Zorbax SB C(18) column. The mobile phase consisted of acetonitrile-water-formic acid (80:20:0.2, v/v/v). Detection was performed on a triple quadrupole tandem mass spectrometer by selected reaction monitoring (SRM) mode via electrospray ionization (ESI) source. The method had a lower limit of quantification of 0.10 ng/ml. The calibration curve was demonstrated to be linear over the concentration range of 0.10-50.0 ng/ml. The assay was specific, accurate (percentage deviations from nominal concentrations were within +/-2.5%), precise (intra- and inter-day relative standard deviation (R.S.D.) <7%). The validated method was successfully applied to the determination of meloxicam in human plasma collected up to 180 h after a transdermal administration of 30 mg meloxicam for evaluation of the pharmacokinetics.
建立了一种高灵敏度和高选择性的液相色谱-串联质谱（LC-MS-MS）法，用于测定人血浆中低浓度的美洛昔康。通过甲醇一步蛋白沉淀进行简单的样品制备后，美洛昔康和内标吡罗昔康在Zorbax SB C(18)柱上进行色谱分离。流动相由乙腈-水-甲酸（80:20:0.2，v/v/v）组成。在三重四极杆串联质谱仪上通过电喷雾电离（ESI）源的选择反应监测（SRM）模式进行检测。该方法的定量下限为0.10 ng/ml。校准曲线在0.10-50.0 ng/ml的浓度范围内呈线性。该测定方法具有特异性、准确性（与标称浓度的百分比偏差在+/-2.5%以内）、精密度（日内和日间相对标准偏差（R.S.D.）<7%）。经过验证的方法成功应用于经皮给予30 mg美洛昔康后180小时内采集的人血浆中美洛昔康的测定，以评估其药代动力学。
