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Determination of gemcitabine and its metabolite in human plasma using high-pressure liquid chromatography coupled with a diode array detector

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文摘 AIM: To establish a high pressure liquid chromatography (HPLC) method for determination of the concentration of gemcitabine (dFdC) and its metabolite (dFdU) in human plasma. METHODS: Plasma 1.0 mL spiked with floxuridine as an internal standard was extracted with 3.0 mL of methanol-acetonitrile (v/v, 1:9). The supernatant was evaporated at 60 oC and the residue was reconstituted with 0.5 mL of the solution used as the mobile phase. After centrifugation, 50 μL of the supernatant was injected into the HPLC system. Separation was achieved on a C18 (4.6 mm×250 mm, 5 μm) column at 25 oC with the flow rate of the mobile phase set to 0.8 mL/min. The compounds were detected at 268 nm. The mobile phase consisted of 40.0 mmol/L acetate ammonium buffer solution (pH 5.5) and acetonitrile (v/v, 97.5:2.5). RESULTS: The linear range was 0.20-10.0 mg/L (r=0.9999) for dFdC and 0.50-50.0 mg/L (r=0.9999) for dFdU. The limit of detection (LOD) was 0.10 mg/L for dFdC and 0.25 mg/L for dFdU, while the limit of quantification (LOQ) was 0.20 mg/L (RSD<10 %) for dFdC and 0.50 mg/L (RSD<3 %) for dFdU. The average recovery of dFdC and dFdU by this method were 103.3 % and 98.7 %, respectively. For intra-day and inter-day, the corresponding standard deviations of the measurements of dFdC and dFdU were both less than 5.5 %. CONCLUSION: An analytical method was established to measure the concentrations of dFdC and dFdU in human plasma and was effectively applied to the dFdC and dFdU pharmacokinetic studies of 8 Chinese patients with malignant tumors.
来源 Acta Pharmacologica Sinica ,2004,25(12):1584-1589 【核心库】
关键词 high pressure liquid chromatography ; gemcitabine ; deoxycytidine ; floxuridine
地址

1. College of Pharmaceutical Sciences, Zhejiang University, Hangzhou, 310031  

2. Zhejiang Cancer Hospital, Hangzhou, 310022

语种 英文
文献类型 研究性论文
ISSN 1671-4083
学科 药学
基金 浙江省教育厅项目
文献收藏号 CSCD:1841668

参考文献 共 14 共1页

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引证文献 4

1 林能明 静脉注射后吉西他滨及其代谢产物在人体内的药动学研究 中国药学杂志,2005,40(14):1089-1092
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2 郭燕萍 用HPLC法测定大鼠血浆中吉西他滨的浓度 药学服务与研究,2009,9(4):301-303
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