Kollroser Manfred, Schober Caroline
Institute of Forensic Medicine, Karl-Franzens University Graz, Austria.
J Chromatogr B Analyt Technol Biomed Life Sci. 2002 Jan 25;766(2):219-26. doi: 10.1016/s0378-4347(01)00469-8.
A sensitive and specific high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS-MS) method has been developed for the simultaneous determination of amiodarone and desethylamiodarone in human plasma. After the addition of the internal standard tamoxifen, plasma samples were extracted using Oasis MCX solid-phase extraction cartridges. The compounds were separated on a 5 microm Symmetry C18 (Waters) column (150 x 3.0 mm, internal diameter) with a mobile phase of acetonitrile-0.1% forrmic acid (46:54, v/v) at a flow-rate of 0.5 ml/min. The overall extraction efficiency was more than 89% for both compounds. The assay was sensitive down to 1 microg/l for amiodarone and down to 0.5 microg/l for desethylamiodarone. Within-run accuracies for quality-control samples were between 95 and 108% of the target concentration, with coefficients of variation <8%. The proposed method enables the unambiguous identification and quantitation of amiodarone and desethylamiodarone in both clinical and forensic specimens.
已开发出一种灵敏且特异的高效液相色谱 - 电喷雾电离 - 串联质谱法（HPLC - ESI - MS - MS），用于同时测定人血浆中的胺碘酮和去乙基胺碘酮。加入内标他莫昔芬后，血浆样品用Oasis MCX固相萃取柱进行萃取。化合物在5微米的Symmetry C18（沃特世）柱（150×3.0毫米，内径）上分离，流动相为乙腈 - 0.1%甲酸（46:54，v/v），流速为0.5毫升/分钟。两种化合物的总体萃取效率均超过89%。该测定法对胺碘酮的检测限低至1微克/升，对去乙基胺碘酮的检测限低至0.5微克/升。质量控制样品的批内准确度在目标浓度的95%至108%之间，变异系数<8%。所提出的方法能够明确鉴定和定量临床及法医标本中的胺碘酮和去乙基胺碘酮。
