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采用液相色谱-电喷雾串联质谱法测定人血中的酸性和中性治疗药物。

Determination of acidic and neutral therapeutic drugs in human blood by liquid chromatography-electrospray tandem mass spectrometry.

机构信息

Section for Toxicology and Drug Analysis, Department of Forensic Medicine, Aarhus University, Brendstrupgaardsvej 100, 8200 Aarhus N, Denmark.

出版信息

Forensic Sci Int. 2011 Mar 20;206(1-3):119-26. doi: 10.1016/j.forsciint.2010.07.016. Epub 2010 Aug 12.

DOI:10.1016/j.forsciint.2010.07.016
PMID:20708359
Abstract

A liquid chromatography-tandem mass spectrometry method using pneumatically assisted electrospray ionisation (LC-ESI-MS/MS) was developed for the simultaneous determination of paracetamol, naproxen, ibuprofen, etodolac, diclofenac, salicylic acid, lamotrigine, carbamazepine, 10-OH-carbazepine, phenytoin, phenobarbital, barbital, cyclobarbital, pentobarbital, amobarbital and caffeine in human live and post-mortem whole blood. The blood proteins were precipitated in a mixture of methanol and acetonitrile, and the extract was purified by ultrafiltration. The separation was performed on an ether-linked phenyl column with polar endcapping, and both negative and positive ESI were applied. Matrix-matched standards were used for calibration. The relative intra-laboratory reproducibility standard deviations were, in general, better than 8% at concentrations in the therapeutic range. The mean true recoveries were in the range 92-101% for the live blood and 84-101% for the post-mortem blood.

摘要

建立了一种采用气动辅助电喷雾电离(LC-ESI-MS/MS)的液相色谱-串联质谱法,用于同时测定人活全血和死后全血中的扑热息痛、萘普生、布洛芬、依托度酸、双氯芬酸、水杨酸、拉莫三嗪、卡马西平、10-羟基卡马西平、苯妥英、苯巴比妥、戊巴比妥、环己巴比妥、戊巴比妥、苯巴比妥和咖啡因。将血液蛋白沉淀在甲醇和乙腈的混合物中,并用超滤法对提取物进行纯化。分离在带有极性封端的醚键合苯基柱上进行,同时应用正负 ESI。使用基质匹配标准品进行校准。在治疗范围内的浓度下,通常,相对实验室内重现性标准偏差小于 8%。活血的平均真实回收率范围为 92-101%,死后血的平均真实回收率范围为 84-101%。

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