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顶空气相色谱法测定盐酸格拉司琼中硫酸二甲酯残留量
引用本文:邓桂凤,姚彤炜. 顶空气相色谱法测定盐酸格拉司琼中硫酸二甲酯残留量[J]. 浙江大学学报(医学版), 2008, 37(2): 156-158. DOI: 10.3785/j.issn.1008-9292.2008.02.009
作者姓名:邓桂凤  姚彤炜
作者单位:浙江大学药学院药物分析与药物代谢研究室,浙江,杭州,310058
摘    要:目的建立盐酸格拉司琼中硫酸二甲酯残留量的测定法.方法采用顶空气相色谱法,载气为氮气,FID检测器,色谱柱为Angilent INNOWAX毛细管柱,柱温50℃,单点对照法检测盐酸格拉司琼中硫酸二甲酯的含量.结果盐酸格拉斯琼中硫酸二甲酯未检出.且在同一色谱条件下,硫酸二甲酯的保留时间与可能存在的其它残留溶剂乙醇、乙酸乙酯、异丙醇、二氯甲烷和氯仿等的保留时间不同,方法的专属性良好;测得硫酸二甲酯的检出限为0.0016%.结论建立的方法能有效控制盐酸格拉司琼中硫酸二甲酯的残留量.

关 键 词:格兰塞隆/分析  色谱法  气相  药物残留物/分析  盐酸格拉司琼  有机溶剂残留量  硫酸二甲酯  顶空气  色谱法测定  盐酸  格拉司  琼中  硫酸二甲酯  残留量  gas chromatography  granisetron hydrochloride  residual  sulphate  控制  专属性  氯仿  二氯甲烷  异丙醇  乙酸乙酯  乙醇  残留溶剂  存在
文章编号:1008-9292(2008)02-0156-03
修稿时间:2007-12-14

Determination of dimethyl sulphate residual in granisetron hydrochloride by headspace gas chromatography
DENG Gui-feng,YAO Tong-wei. Determination of dimethyl sulphate residual in granisetron hydrochloride by headspace gas chromatography[J]. Journal of Zhejiang University. Medical sciences, 2008, 37(2): 156-158. DOI: 10.3785/j.issn.1008-9292.2008.02.009
Authors:DENG Gui-feng  YAO Tong-wei
Affiliation:Department of Pharmaceutical Analysis and Drug Metabolism, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China.
Abstract:OBJECTIVE: To develop a headspace gas chromatography method for determining dimethyl sulphate residual in granisetron hydrochloride. METHODS: An Angilent INNOWAX capillary column with nitrogen gas as carrier and FID as detector was applied in this study. Dimethyl sulphate was tested under a constant column temperature. RESULT: Dimethyl sulphate had different retention time from other organic solvents such as alcohol,acetoacetate, isopropanol, dichlormethane and chloroform, which might exist in granisetron hydrochloride. The detection limit of dimethyl sulphate;s was 0.0016%. CONCLUSION: The method can be used for the determination of dimethyl sulphate residual in granisetron hydrochloride.
Keywords:Granisetron/anal  Chromatography  gas  Drug residues/anal  Granisetron hydrochloride  Residual solvent  Dimethyl sulphate  
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