Capillary GC Determination of Fentanyl and Midazolam in Human Plasma

Capillary GC Determination of Fentanyl and Midazolam in Human Plasma
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DOI:
10.1006/mchj.1996.0017
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发表时间:
1996
影响因子:
4.8
通讯作者:
Li Yuansheng;Wu Yutian;Z. Jing;Zhai Zhenxing;Qi Zhanxi;G. Shen;Kong Qinghong;W. Xinhua
Li Yuansheng;Wu Yutian;Z. Jing;Zhai Zhenxing;Qi Zhanxi;G. Shen;Kong Qinghong;W. Xinhua
中科院分区:
化学2区
文献类型:
--
作者:
Li Yuansheng;Wu Yutian;Z. Jing;Zhai Zhenxing;Qi Zhanxi;G. Shen;Kong Qinghong;W. Xinhua

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摘要建立了同时测定人血浆中芬太尼和咪达唑仑的毛细管气相色谱法。以环己烷-异戊醇(197:3)为内标,以芬太尼衍生物为载体,在碱性pH下提取血浆。用硫酸反提,碱提后用己烷再提。有机相在40°C氮气下蒸发,残渣溶解于乙醇中。采用HP-1 (2.65 μm)宽孔毛细管柱(10 m × 0.53 mm),载气n2, N - p检测器,温度255°C。芬太尼和咪达唑仑在0.5 ~ 100和5 ~ 1000 ng/ml范围内呈线性关系,相关系数为0.9998。芬太尼和咪达唑仑的回收率分别为99.5±4.5和99.9±3.2%。组内和组间变异系数小于7%。芬太尼的检出限为0.2 ng/ml,咪达唑仑的检出限为0.5 ng/ml。该方法已应用于治疗药物监测和药代动力学研究。
Abstract A capillary GC method is described for simultaneously measuring fentanyl and midazolam in human plasma. Plasma was extracted at basic pH with cyclohexane–isopentanol (197:3) with Ro21-2212 added as internal standard and fentanyl derivative as carrier. The drug was back-extracted in H 2 SO 4 , and then the extract was made basic and reextracted with hexane. The organic phase was evaporated at 40°C under N 2 and the residue was dissolved in ethanol. A portion was analyzed on a wide-bore capillary column (10 m × 0.53 mm) of HP-1 (2.65 μm), operated at 255°C with N 2 as carrier gas and N–P detector. The calibration graph for fentanyl and midazolam was linear within the respective ranges of 0.5–100 and 5–1000 ng/ml with a correlation coefficient of 0.9998. The recovery of fentanyl and midazolam was 99.5 ± 4.5 and 99.9 ± 3.2%. The coefficient of variation within a run and between runs was less than 7%. The detection limit for fentanyl was 0.2 ng/ml plasma, and for midazolam was 0.5 ng/ml plasma. The method was applied to therapeutic drug monitoring and pharmacokinetic studies.