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人血浆中盐酸多奈哌齐的HPLC-MS测定法(英文)

Quantitation of Donepezil in Human Plasma by HPLC-MS

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【作者】 丁黎郝歆愚李丽敏卞晓洁张胜强

【Author】 DING Li, HAO Xin-Yu, LI Li-Μin, BIAN Xiao-Jie,ZHANG Sheng-Qiang (Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing 210009, China)

【机构】 中国药科大学药物分析教研室中国药科大学药物分析教研室 南京210009南京210009南京210009

【摘要】 目的 :建立人血浆中盐酸多奈哌齐的HPLC MS法。方法 :血样经饱和NaHCO3 碱化后用乙酸乙酯提取 ,进行HPLC MS分析 ,色谱柱为HypersilODS(5μm ,2 50mm× 4 6mm) ,流动相为甲醇 水 三乙胺 冰醋酸 (70∶3 0∶0 3∶0 3 ) ,内标为盐酸非洛普 ,检测离子为m /z 3 80 (多奈哌齐 )、m/z 3 4 4 (内标 ) ,裂解电压为 12 0V。结果 :在 0 2~ 2 0ng/ml范围内多奈哌齐与内标峰面积比值与浓度线性关系良好 (r =0 9996) ,最低可定量浓度为 0 1ng/ml,提取回收率为 87 52 %~ 90 91%。结论 :本实验建立的分析方法灵敏、准确、简便

【Abstract】 AIM and METHOD:A highly sensitive method for quantita tion of donepezil in human plasma was established by using liquid chromatography -electrospray ionization-mass spectrometry (LC-ESI-MS), with phenoprolamine hydrochloride as the internal standard (I.S. ). After alkalizing with saturated sodium bicarbonate, plasma was extracted with e thyl acetate and the extracts were separated by HPLC on a C 18 reversed-ph ase c olumn with methanol-water-acetic acid-triethylamine (70∶30∶03∶03,v/ v ) as mobile phase. LC-ESI-MS was performed in the selected ion monitoring (S IM) mode us in g target ions at m/z 380 for donepezil and m/z 344 for the I.S..RE SULT:Calibra tion curves, which were linear over the range of 02 to 20 ng/ml, were establis hed contemporaneously with the analyses of each batch of samples, along with low (0 2 ng/ml), medium (2 ng/ml) and high (20 ng/ml) quality control samples. The in tra a nd inter-assay variability ranged from 125% to 984% for the low, medium and hig h quality control samples. The extraction recovery of donepezil from plasma was in the range of 875%~919%.CONCLUSION:The method has been us ed successfully to study donepezil pharmacokinetics in human plasma.

【关键词】 盐酸多奈哌齐HPLCMS血浆含量测定
【Key words】 DonepezilHPLC-MSHuman plasmaDetermi nation of content
  • 【文献出处】 中国药科大学学报 ,Journal of China Pharmaceutical University , 编辑部邮箱 ,2004年01期
  • 【分类号】R96
  • 【被引频次】6
  • 【下载频次】225
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