文献类型：期刊文献

中文题名：顶空气相色谱法测定盐酸托莫西汀中有机溶剂残留量的研究

英文题名：Determination of residual organic solvents in tomoxetine hydrochloride by headspace gas chromatography

作者：胡慧廉[1];丁乃立[1];吴莲珍[1]

机构：[1]华东理工大学分析测试中心,上海200237

年份：2007

卷号：26

期号：10

起止页码：76

中文期刊名：分析试验室

外文期刊名：Chinese Journal of Analysis Laboratory

收录：CSTPCD;;北大核心:【北大核心2004】；CSCD:【CSCD2011_2012】；

语种：中文

中文关键词：顶空气相色谱法;盐酸托莫西汀;有机溶剂残留量

外文关键词：Headspace gas chromatography; Tomoxetine hydrochloride; Residual organic solvents

摘要：建立了盐酸托莫西汀中有机溶剂残留量的顶空气相色谱分析方法。选用大口径HP-快速GC残留溶剂柱为分离柱,FID为检测器,外标法进行定量,并对顶空平衡温度、平衡时间、供试品溶液的制备方法对残留有机溶剂测定的影响进行了研究。甲醇、乙醚、正己烷、乙酸乙酯、四氢呋喃的线性范围分别为0.41～8.10μg/mL(r=0.9999)、0.15～3.00μg/mL(r=0.9995)、0.20～4.01μg/mL(r=0.9991)、0.32～6.35μg/mL(r=0.9999)、0.36～7.11μg/mL(r=0.9999);平均回收率范围96.30%～105.47%,精密度RSD(n=6)2.1%～3.7%;检出限分别为0.2、0.008、0.003、0.04、0.04μg/mL。
A method for the determination of five kinds of residual organic solvents in tomoxetine hydrochloride has been developed by headspace gas chromatography. A wide bore HP-fast GC residual solvent column was chosen for separation with FID detector. The external standard method was used for quantitative analysis. Several factors affecting the headspace detennination were studied, including equilibrium temperature, equilibrium time and sample preparation. The standard curves were linear in the range of 0.41 - 8.10 μg/mL （ r = 0.9999） for methanol, 0.15 - 3.00 μg/mL （r =0.9995） for diethyl ether, 0.20-4.01 μg/mL （r =0.9991） for hexane, 0.32-6.35 μg/mL （r = 0.9999） for ethyl acetate and 0.36- 7.11 μg/mL （r = 0.9999） for tetrahydrofuran. The average recoveries for five residual organic solvents were between 96.30% and 105.47 % with RSD （n = 6） of precision in the range of 2.1% - 3.7 %. The detection limits of methanol, diethyl ether, hexane, ethyl acetate and tetrahydrofuran were 0.2, 0.008, 0.003, 0.04 and 0.04 μg/mL respectively.