顶空-气相色谱法同时测定维生素B1片中9种溶剂残留量
Simultaneous Determination of 9 Residual Solvents in Vitamin B1 Tablets by Headspace-Gas Chromatography
余红 1何亚芬 1张继红 1郑露盼1
作者信息
- 1. 上饶市检验检测认证院,江西 上饶 334000
- 折叠
摘要
目的 建立维生素B1 片中甲醇、乙醇、丙酮、甲酸乙酯、乙腈、正己烷、乙酸乙酯、四氢呋喃和正庚烷 9 种残留有机溶剂气相色谱分离测定方法.方法 采用顶空毛细管气相色谱法,6%(V/V)氰丙基苯基-94%(V/V)二甲基聚硅氧烷(DB-624)为固定液的毛细管柱(30 m×0.530 mm×3.00 μm),氢火焰离子化检测器(FID),载气为氮气,溶剂为N,N-二甲基甲酰胺(DMF)∶水(1∶1),按外标法计算残留溶剂的含量.结果 9 种有机溶剂均能有效分离,峰响应与浓度均呈良好线性关系,相关系数r均大于 0.999 64;平均回收率在 92.2%～111.7%(n=9);精密度RSD值在0.3%～1.0%(n=6).结论 该方法分离效果好、灵敏、可靠、准确,适用于维生素B1 片中 9 种溶剂残留量的同时测定.
Abstract
Objective To establish a gas chromatographic separation and determination method for 9 residual organic solvents in vitamin B1 tablets,including methanol,ethanol,acetone,ethyl formate,acetonitrile,n-hexane,ethyl acetate,tetrahydrofuran and n-heptane.Methods Using headspace capillary gas chromatography,a capillary column with 6%(V/V)cyanopropylphenyl-94%(V/V)dimethylpolysiloxane(DB-624)as the stationary phase was used(30 m×0.530 mm×3.00 μm),The detector was FID,the carrier gas was nitrogen,and the solvent was DMF:water(1:1).The residual solvent content was calculated using the external standard method.Results All 9 organic solvents were effectively separated and showed a good linear relationship,with a correlation coefficient greater than 0.999 64;the average recovery rate ranges from 92.2%-111.7%(n=9);the precision RSD was within 0.3%-1.0%(n=6).Conclusion This method has good separation effect,sensitivity,reliability,and accuracy,and is suitable for the simultaneous determination of 9 residual solvents in vitamin B1 tablets.
关键词
维生素B1片/顶空进样/毛细管气相色谱法/残留溶剂测定Key words
Vitamin B1 tablets/Headspace injection/Capillary gas chromatography/Determination of residual solvents引用本文复制引用
出版年
2024
NETL
NSTL
万方数据