Kaunzinger Astrid, Baumeister Alwin, Cuda Klaus, Häring Norbert, Schug Barbara, Blume Henning H, Raddatz Klaus, Fischer Gerhard, Schubert-Zsilavecz Manfred
Institut of Pharmaceutical Chemistry, University Frankfurt, Marie-Curie-Str. 9, D-60439, Frankfurt, Germany.
J Pharm Biomed Anal. 2002 May 15;28(3-4):729-39. doi: 10.1016/s0731-7085(01)00674-4.
A sensitive, specific, accurate, fast and reproducible GC/MS-method for the quantitative determination of 11-keto-boswellic acid in human plasma using 18alpha-glycyrrhetinic acid as the internal standard was developed and validated. 11-Keto-boswellic acid and the internal standard were separated from acidified plasma by liquid/liquid extraction. The extracted samples were methylated and analyzed by GC/MS in the negative ion chemical ionization mode (NICI) and selected ion monitoring (SIM). The total run time was 8 min between injections. The assay described in this paper demonstrates a validated lower limit of quantification of 0.0100 microg/ml using 1 ml of plasma. The calibration curves are linear in the measured range between 10.0 and 2000 ng/ml plasma. The overall precision (expressed as CV) and accuracy (expressed as bias) for all concentrations of quality controls and standards is better than 15%. No indications were found for possible instabilities of 11-keto-boswellic acid in plasma, in whole blood, in the extraction solvent or after repeated thawing/freezing cycles. The recovery of the extraction method is calculated as 84%. The assay was applied successfully to determine the plasma level of 11-keto-boswellic acid in a clinical pilot study.
建立并验证了一种灵敏、特异、准确、快速且可重现的气相色谱/质谱法（GC/MS），该方法以18α-甘草次酸为内标，用于定量测定人血浆中的11-酮基-乳香酸。11-酮基-乳香酸和内标通过液-液萃取从酸化血浆中分离出来。萃取后的样品进行甲基化处理，然后采用气相色谱/质谱在负离子化学电离模式（NICI）和选择离子监测（SIM）下进行分析。两次进样之间的总运行时间为8分钟。本文所述的测定方法显示，使用1 ml血浆时，验证后的定量下限为0.0100 μg/ml。校准曲线在10.0至2000 ng/ml血浆的测量范围内呈线性。所有浓度的质量控制品和标准品的总体精密度（以CV表示）和准确度（以偏差表示）均优于15%。未发现11-酮基-乳香酸在血浆、全血、萃取溶剂中或经过反复冻融循环后可能存在不稳定性的迹象。萃取方法的回收率计算为84%。在一项临床初步研究中，该测定方法成功应用于测定11-酮基-乳香酸的血浆水平。
