中国药房2017，Vol.28Issue(24)：3426-3429,4.DOI:10.6039/j.issn.1001-0408.2017.24.33
顶空毛细管气相色谱法同时测定阿瑞匹坦原料药中6种有机溶剂的残留量
Simultaneous Determination of 6 Residual Organic Solvents in Aprepitant Raw Material by Headspace Capillary GC
摘要
Abstract
OBJECTIVE:To establish a method for simultaneous determination of 6 residual organic solvents in aprepitant raw material as methanol,ethanol,acetone,isopropyl alcohol,methyl tert-butyl ether and tetrahydrofuran.METHODS:Headspace capillary gas chromatography was adopted.The determination was performed on DB-624 capillary column using temperature programming.The temperature of injector port was 180 ℃,and flame ionization detector was used with temperature of 260 ℃.Nitrogen was used as carrier gas with flow rate 3.0 mL/min.The spilt ratio was 5 ∶ 1,and head-space injection volume was 1.0 mL.The head-space equilibrium temperature was set at 80 ℃,and equilibrium time was 40 min.RESULTS:The linear ranges of methanol,ethanol,acetone,isopropyl alcohol,methyl tert-butyl ether,tetrahydrofuran were 6.052-605.232 μ g/mL (r=0.999 9),9.987-998.718 μg/mL(r=0.999 9),9.998-999.768 μg/mL(r=0.999 8),9.986-998.634 μg/mL(r=0.999 9),9.991-999.090 μg/mL (r=0.999 7),1.461-146.133 μg/mL(r=0.999 5),respectively.The limits of quantitation were 1.782 1,2.079 0,0.749 8,1.777 8,0.223 1,0.607 0 μg/mL;the limits of detection were 0.594 0,0.693 0,0.249 9,0.592 6,0.074 4,0.202 3 μg/mL,respectively.RSD of precision test was lower than 2.0％.Only acetone and isopropyl alcohol were detected in stability test and reproducibility tests,RSD＜2.0％.Their recoveries were 99.34-100.75％ (RSD=0.52％,n=9),98.20％-100.24％ (RSD=0.69％,n=9),98.07％-100.07％ (RSD=0.84％,n=9),99.86％-101.32％ (RSD=0.58％,n=9),97.87％-104.02％ (RSD=2.13％,n=9),98.26 ％-100.58 ％ (RSD =0.75 ％,n =9),respectively.CONCLUSIONS:The established method is simple,accurate and reproducible,and can be used for simultaneous determination of 6 residual organic solvents in aprepitant raw material.关键词
顶空毛细管气相色谱法/阿瑞匹坦/有机溶剂/残留量Key words
Headspace capillary gas chromatography/Aprepitant/Organic solvent/Residual分类
医药卫生引用本文复制引用
郑瑞凤,杨晨,任凤英,贾红倩,冉琳,秦其辉,苟小军,冯菊..顶空毛细管气相色谱法同时测定阿瑞匹坦原料药中6种有机溶剂的残留量[J].中国药房,2017,28(24):3426-3429,4.基金项目
药食同源植物资源开发四川省高校重点实验室开放基金(No.10Y201608) （No.10Y201608）
成都大学校青年基金(No.2015XJZ08) （No.2015XJZ08）
