顶空毛细管气相色谱法测定盐酸洛哌丁胺中残留溶剂
投稿时间:2012-03-18  修订日期:2012-07-06  点此下载全文
引用本文:胡猛慎,洪志玲,黄剑英.顶空毛细管气相色谱法测定盐酸洛哌丁胺中残留溶剂[J].药学实践杂志,2012,30(6):454~456
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作者单位E-mail
胡猛慎 厦门市药品检验所, 福建 厦门 361012  
洪志玲 厦门市药品检验所, 福建 厦门 361012 xmyjh_lwtx@163.com 
黄剑英 厦门市药品检验所, 福建 厦门 361012  
中文摘要:目的 建立了顶空毛细管气相色谱法测定盐酸洛哌丁胺中残留溶剂的方法。方法 以氮气为载气,氢火焰离子化检测器(FID)检测,色谱柱为DB-624毛细管柱(30 m×0.32 mm×0.25 μm),采用程序升温,顶空进样,顶空平衡温度为100℃,平衡时间25 min。对盐酸洛哌丁胺中甲醇、异丙醇、正己烷、乙酸乙酯、四氢呋喃、氯仿、甲基异丁酮、甲苯、苯这9种有机溶剂残留进行检测。结果 在试验条件下实现了各组分的分离。甲醇、异丙醇、正己烷、乙酸乙酯、四氢呋喃、氯仿、甲基异丁酮、甲苯、苯在所考察的浓度范围内,线性关系、精密度均良好。各组分平均回收率95.2%~102.3%,RSD 0.8%~2.9%。结论 该方法简便、准确,可用于盐酸洛哌丁胺中残留溶剂的测定。
中文关键词:顶空气相色谱法  盐酸洛哌丁胺  残留溶剂测定
 
Determination of residue organic solvents in Loperamide Hydrochloride by headspace capillary gas chromatography
Abstract:Objective To develop a method of headspace capillary gas chromatography for determining residual organic solvents in loperamide hydrochloride. Methods The carrier gas was nitrogen and FID as detector. The nine organic solvents including methanol, isopropanol, n-hexane, ethyl acetate, tetrahydrofuran, chloroform, methyl isobutyl ketone, toluene, benzene were separated on a DB-624 capillary column(30 m×0.32 mm×0.25 μm)by programmable increased temperature and headspace gas chromatography. Results The nine organic solvents were separated and each of them showed linear relationship in the concentration range measured. The recoveries and RSDs were in range from 95.2% to 102.3% and 0.8% to 2.9%, respectively. Conclusion The method was simple, accurate and reproducible.
keywords:head-space gas chromatography  Loperamide hydrochloride, determination of residual solvents
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