Determination of 11-keto-boswellic acid in human plasma

被引:21
作者
Kaunzinger, A
Baumeister, A
Cuda, K
Häring, N
Schug, B
Blume, HH
Raddatz, K
Fischer, G
Schubert-Zsilavecz, M
机构
[1] Univ Frankfurt, Inst Pharmaceut Chem, D-60439 Frankfurt, Germany
[2] AAI Deutschland GmbH & Co KG, D-89231 Neu Ulm, Germany
[3] SocraTec R&D GmbH, D-61440 Oberursel, Germany
[4] RP Scherer GmbH & Co KG, D-69412 Eberbach, Germany
关键词
11-keto boswellic acid; human plasma; quantitative determination; GC/MS;
D O I
10.1016/S0731-7085(01)00674-4
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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 mug/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. (C) 2002 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:729 / 739
页数:11
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