Quantitative determination of rocuronium in human plasma by liquid chromatography-electrospray ionization mass spectrometry
Quantitative determination of rocuronium in human plasma by liquid chromatography-electrospray ionization mass spectrometry
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DOI：
10.1016/s0021-9673(00)01164-x
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发表时间：
2001-02-23
影响因子：
4.1
通讯作者：
Aubagnac, JL
中科院分区：
文献类型：
--
作者：
Farenc, C;Enjalbal, C;Aubagnac, JL
液相色谱 - 电喷雾电离质谱法（LC - ESI - MS）用于人血浆中神经肌肉阻滞剂罗库溴铵的定量分析。维拉帕米用作内标。在进行LC - MS分析之前，将带正电荷的铵化合物与碘化物进行离子配对后，对样品进行二氯甲烷液 - 液萃取。优化的条件包括：在Symmetry Shield RP - 18柱（50×2.1 mm，3.5 µm）上进行分离，采用15分钟的梯度洗脱，流动相为含0.1%三氟乙酸的水和乙腈，乙腈的比例从10%到90%，流速为250 µl/min。标准品的线性检测响应在25到2000 ng/ml范围内。罗库溴铵的萃取回收率平均为59%，内标的萃取回收率为83%。使用500 µl血浆时，定量限（LOQ）为25 ng/ml。精密度在1.3%到19%（LOQ）之间，准确度在92%到112%之间。在血浆样品中，在20℃和4℃条件下，罗库溴铵在生理pH值下稳定4小时；在 - 30℃冷冻时，至少稳定75天。该方法适用于人体药代动力学研究中采集的样品分析。（C）2001 Elsevier Science B.V.保留所有权利。
Liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) was used for the quantification of the neuromuscular blocking agent rocuronium in human plasma. Verapamil was used as internal standard. The samples were subjected to a dichloromethane liquid-liquid extraction after ion pairing of the positively charged ammonium compound with iodide prior to LC-MS. Optimized conditions involved separation on a Symmetry Shield RP-18 column (50X2.1 mm, 3.5 mum) using a 15-min gradient from 10 to 90% acetonitrile in water containing 0.1% trifluoroacetic acid at 250 mul/min. Linear detector responses for standards were observed from 25 to 2000 ng/ml. The extraction recovery averaged 59% for rocuronium and 83% for the internal standard. The limit of quantification (LOQ), using 500 mul of plasma, was 25 ng/ml. Precision ranged from 1.3 to 19% (LOQ), and accuracy was between 92 and 112%. In plasma samples, at 20 and 4 degreesC, rocuronium was stable at physiological pH for 4 h; frozen at - 30 degreesC it was stable for at least 75 days. The method was found suitable for the analysis of samples collected during pharmacokinetic investigations in humans. (C) 2001 Elsevier Science B.V. All rights reserved.