Simultaneous extraction and quantitation of fentanyl and norfentanyl from primate plasma with LC/MS detection

Simultaneous extraction and quantitation of fentanyl and norfentanyl from primate plasma with LC/MS detection
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DOI:
10.1016/s0731-7085(03)00652-6
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发表时间:
2004-02-18
影响因子:
3.4
通讯作者:
Hunter, RP
Hunter, RP
中科院分区:
医学3区
文献类型:
--
作者:
Koch, DE;Isaza, R;Hunter, RP

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The quantitation of both fentanyl and its desalkyl metabolite, norfentanyl, in plasma using LC/MS has not been previously described. The detection and quantitation of fentanyl and norfentanyl was achieved using LC/MS detection. The liquid-liquid extraction used toluene as the organic phase. Chromatography was carried out using a Zirchrom-PBD (50 mm x 2.1 mm, 3 mum) column with a mobile phase of acetonitrile-ammonium acetate (10 mM), citrate (0.1 mM, pH 4.4) (45:55, v/v) with a flow rate of 0.3 ml/min. Mass spectroscopy detection was performed using ESI in the positive mode. The LOQ for fentanyl was 25 pg/ml and norfentanyl was 50 pg/ml. For the concentrations of 75, 250, and 750 pg/ml, respectively, fentanyl had inter-day precisions of 6.6. 7.2. and 6.6% with accuracies of 4.0, 5.1, and 5.1% and intra-day precisions of 1.6, 1.9, and 1.9% with accuracies of 11.6. 9.4. and 8.4%. and norfentanyl had inter-day precisions of 7.4, 0.3, and 0.7% with accuracies of 9.1, 8.8, and 12.3% and intra-day precisions of 5.3. 1.4, and 0.1% with accuracies of 10.9, 8.9, and 12.8%. The recoveries of fentanyl were 85, 92, and 75% and of norfentanyl were 40, 49, and 46% at the 75, 250, and 750 pg/ml concentrations, respectively. (C) 2003 Elsevier B.V. All rights reserved.