HPLC Determination of An Illicit Additive Ribavirin in Anti-Viral Oral Liquor with Column Switching
摘 要
提出了由双泵单阀的驱动系统和双柱(预处理柱和分析柱)切换的分析系统所组成的色谱分析流程并应用于测定抗病毒口服液中非法添加物利巴韦林.样品离心后取上清液直接进样于C18预处理柱,水作为预处理流动相;用0.3 g·L-1磷酸二氢钠溶液(分析流动相)将保留在预处理柱上的药物冲入Kromasil C18分析柱(250 mm×4.6 mm,5 μm)进行测定.方法集样品净化和色谱分析一次连续进行,测定条件下无干扰.检测波长205.6 nm,药物的质量浓度在0.4~40.0 mg·L-1范围内呈线性(r=0.999 2),检出限(S/N=3)为0.08 mg·L-1,加标回收率分别为98.32%,98.45%,99.45%.
Abstract
An flow circuit of HPLC analysis,consisting of the driving system(bi-pump and single value system) and the column switching system(pretreatment column and analytical column) was designed and applied to the determination of anillicit additive,ribavirin,in antiviral oral liquor.The oral liquor sample was centrifuged and diluted with 0.3 g·L-1 NaH2PO4 solution to a definite volume.A aliquot of the sample was introduced into the pretreatment C18 column(mode A of the flow circuit),where the purification process was performed.Mobile phase consisting of CH3OH and H2O,in the ratio of 1+3,was used in the pretreatment column.Drug components adsorbed on the pretreatment column was eluted directly into the analytical kromasil C18 column(250 mm×4.6 mm,5 μm) with 0.3 g·L-1 NaH2PO4 solution as mobile phase by switching to mode B of the flow circuit,and ribavirin was determined with UV-detector at 205.6 nm.Linearity range was found in the range of 0.4-40.0 mg·L-1,with a detection limit(S/N=3) of 0.08 mg·L-1.Test for recovery was made at 3 different concentration levels of 1.0,5.0 and 10.0 mg·L-1 of ribavirin,giving average values of recovery(n=5) 98.32%,98.45% and 99.45% respectively.
中图分类号 O657.7
所属栏目 工作简报
基金项目 福建省科技厅科技三项经费资助课题(项目编号:K04062)
收稿日期 2006/12/15
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备注程永华(1964-),女,湖南南阳人,副教授,从事分析化学研究.
引用该论文: CHENG Yong-hua,HU Juan. HPLC Determination of An Illicit Additive Ribavirin in Anti-Viral Oral Liquor with Column Switching[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(6): 545~547
程永华,胡娟. 柱切换-高效液相色谱法测定抗病毒口服液中非法添加利巴韦林[J]. 理化检验-化学分册, 2008, 44(6): 545~547
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【3】孙立新,唐虹.RP-HPLC法测定板蓝根、大青叶中靛蓝、靛玉红的含量[J].沈阳药科大学学报,2000,17(3):191-193.
【4】刘根成,都恒青,梁 力.反相高效液相色谱法测定地黄中梓醇的含量[J].中草药,1992,23(2):71-73.
【5】杨永钢,孙国祥.石菖蒲中α,β-细辛醚含量的测定[J].沈阳药科大学学报,2003,20(2):116-118.
【6】郭玫,郭力.石菖蒲中α,β-细辛醚含量的测定[J].成都中医药大学学报,1999,22(4):26-27.
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