Farrar Henry, Letzig Lynda, Gill Michael
Section on Pediatric Clinical Pharmacology, University of Arkansas for Medical Sciences, Arkansas Children's Hospital Research Institute, 800 Marshall Street, Little Rock, AR 72202-3591, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2002 Nov 25;780(2):341-8. doi: 10.1016/s1570-0232(02)00543-3.
A simple, rapid method of determining the ibuprofen concentration in small volumes of human plasma (50 microl) by HPLC was developed. The sample was prepared for injection using a solid-phase extraction method, with naproxen as the internal standard. A 96-well extraction plate was used, easing sample preparation and allowing the simultaneous extraction of multiple plasma samples directly into the HPLC injection vials. Samples were stable at room temperature for at least 48 h prior to injection. The HPLC method used an ultraviolet detector with a 5-min run time and measured concentrations across the range typically seen with the clinical use of this drug. The calibration curve was linear across the concentration range of 0.78-100 microg/ml with a limit of quantitation (LOQ) of 1.56 microg/ml. The coefficient of variation for intra-day and inter-day precision was 6% or less with accuracies within 2% of the nominal values for low (4.5 microg/ml), medium (40 microg/ml) and high (85 microg/ml) ibuprofen concentrations. For ibuprofen concentrations at the LOQ, the intra-day and inter-day precision and accuracy were within 10 and 15%, respectively. Recovery was 87% or greater for ibuprofen. This method was used to analyze plasma samples for unknown ibuprofen concentrations in bioequivalence and limited food effect studies of different formulations of ibuprofen. Thus, this method has been fully validated and used in the analysis of unknown plasma samples for ibuprofen.
开发了一种通过高效液相色谱法（HPLC）测定少量人血浆（50微升）中布洛芬浓度的简单、快速方法。采用固相萃取法制备供注射用的样品，以萘普生作为内标。使用96孔萃取板，简化了样品制备过程，并允许将多个血浆样品直接同时萃取到HPLC进样瓶中。样品在注射前于室温下至少稳定48小时。该HPLC方法使用紫外检测器，运行时间为5分钟，可测量该药物临床使用中常见浓度范围内的浓度。校准曲线在0.78 - 100微克/毫升的浓度范围内呈线性，定量限（LOQ）为1.56微克/毫升。日内和日间精密度的变异系数为6%或更低，低（4.5微克/毫升）、中（40微克/毫升）和高（85微克/毫升）布洛芬浓度的准确度在标称值的2%以内。对于LOQ浓度的布洛芬，日内和日间精密度及准确度分别在10%和15%以内。布洛芬的回收率为87%或更高。该方法用于分析生物等效性研究及布洛芬不同制剂的有限食物效应研究中未知布洛芬浓度的血浆样品。因此，该方法已得到充分验证，并用于分析未知的布洛芬血浆样品。
