详细信息
用GC-FID和GC-TOF-MS方法分析α-硫辛酸中有机溶剂残留量
Determination of residual solvents in α-lipoic acid by GC-FID and GC-TOF-MS
文献类型:期刊文献
中文题名:用GC-FID和GC-TOF-MS方法分析α-硫辛酸中有机溶剂残留量
英文题名:Determination of residual solvents in α-lipoic acid by GC-FID and GC-TOF-MS
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:2006
卷号:25
期号:7
起止页码:102
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:气相色谱法;色-质联用;残留有机溶剂;α-硫辛酸
外文关键词:Gas chromatography; GC-MS; Residual organic solvents; α-lipoic acid
摘要:采用GC-TOF-MS鉴定残留有机溶剂,以HP-5毛细管柱为分离柱,FID为检测器,正辛醇为溶剂,外标法进行定量。乙醚、异丙醚的线性范围分别为34.4~344.0μg/mL(r=0.9999),23.0~230.0μg/mL(r=0.9999);方法精密度和稳定性试验RSD(n=6)均〈1%;平均回收率范围98.1%~100.7%,RSD0.75~2.7%;检出限分别为0.1,0.08μg/mL。
A method for the determination of residual organic solvents in α-lipoic acid has been developed by gas chromatography. There were two kinds of residual solvents in α-lipoic acid identified by GC-TOF-MS. The analysis was performed on HP-5 capillary column with 1-octanol as solvent. The external standard method was used for quantitative analysis. The standard curves were linear in the range of 34.4 - 344.0 μg/mL ( r = 0.9999) for diethyl ether and 23.0 - 230.0 μg/mL ( r = 0.9999) for di-iso-propyl ether. The relative standard deviations ( n = 6) of precision and stability were less than 1%. The average recoveries for both residual solvents were between 98.1% and 100.7% with RSD in the range of 0.75 % - 2.7 %. The detection limits were 0.1μg/mL for diethyl ether and 0.08 μg/mL for di- iso-propyl ether.
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