Ramakrishna N V S, Vishwottam K N, Wishu S, Koteshwara M
Biopharmaceutical Research, Suven Life Sciences Ltd., Serene Chambers, Road # 7, Banjara Hills, Hyderabad 500034, India.
J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Feb 25;816(1-2):215-21. doi: 10.1016/j.jchromb.2004.11.034.
A simple, sensitive and specific HPLC method with UV detection (284 nm) was developed and validated for quantitation of Etoricoxib in human plasma, the newest addition to the group of nonsteroidal anti-inflammatory drugs-a highly selective cyclooxygenase-2 inhibitor. Following a single-step liquid-liquid extraction with diethyl ether/dichloromethane (70/30, v/v), the analyte and internal standard (Zaleplon) were separated using an isocratic mobile phase of water/acetonitrile (58/42, v/v) on reverse phase Waters symmetry C(18) column. The lower limit of quantitation was 5 ng/mL, with a relative standard deviation of less than 20%. A linear range of 5-2500 ng/mL was established. This HPLC method was validated with between- and within-batch precision of 4.1-5.1% and 1.1-2.4%, respectively. The between- and within-batch bias was -3.8-4.7% and -0.6-9.4%, respectively. Frequently coadministered drugs did not interfere with the described methodology. Stability of Etoricoxib in plasma was >90%, with no evidence of degradation during sample processing (autosampler) and 30 days storage in a freezer. This validated method is sensitive and simple with between-batch precision of <6% and was used in pharmacokinetic studies.
开发并验证了一种简单、灵敏且特异的高效液相色谱法（HPLC），采用紫外检测（284 nm）对人血浆中的依托考昔进行定量分析。依托考昔是最新加入非甾体抗炎药组的药物——一种高选择性环氧化酶-2抑制剂。采用乙醚/二氯甲烷（70/30，v/v）进行单步液-液萃取后，在反相沃特世对称C(18)柱上，使用水/乙腈（58/42，v/v）的等度流动相分离分析物和内标（扎来普隆）。定量下限为5 ng/mL，相对标准偏差小于20%。建立了5-2500 ng/mL的线性范围。该HPLC方法经批次间和批次内精密度验证，分别为4.1-5.1%和1.1-2.4%。批次间和批次内偏差分别为-3.8-4.7%和-0.6-9.4%。常用的合并用药不干扰所述方法。依托考昔在血浆中的稳定性>90%，在样品处理（自动进样器）过程中无降解迹象，在冷冻条件下储存30天也无降解。这种经过验证的方法灵敏且简单，批次间精密度<6%，已用于药代动力学研究。
