气相色谱法测定格列本脲胶囊中二甲基甲酰胺的含量

Determination of N,N dimethyl formamide in micronazed gilibenclamide capsules by gas chromatography

目的 测定格列本脲胶囊中残留有机溶剂二甲基甲酰胺的含量。方法 采用气相色谱法 ,氢火焰离子化检测器 (FID) ,以二甲基亚砜为溶剂 ,四氢呋喃为内标 ,采用毛细管柱 ,以 10 0 %二甲基聚硅氧烷为固定相 ,柱温 15 0℃维持 14min ,以 40℃·min-1的速率升温至 2 0 0℃ ,维持 12min ,实现了各组分的基线分离。结果 3批格列本脲胶囊中二甲基甲酰胺的残留量均低于限量 (0 .0 88% )。结论 经方法学试验验证 ,该方法灵敏、准确、可信 ,适用于本品有机溶剂残留量的测定。

OBJECTIVE To determine the content of N,N dimethyl formamide,the residual organic volatile solvents,in micronazed gilibenclamide capsules.METHODS Dissolved in dimethyl sulphoxide,2 μL sample solution was injected on a DB 1 (100% dimethyl polysiloxane) sillica capillary column using nitrogen as the carrier gas.Keep the initial temperature at 150℃ for 14 min,then it was raised to 200℃ at the rate of 40 ℃·min -1 ,sustained for 12 min.The injection port and FID detector were 210℃ and 240℃.Under this condition,N,N dimethyl formamide and the internal standard tetrahydrofuran were separated completeh.RESULTS The linear range of N,N dimethyl formamide was 35.19～28.15 μg·mL -1 ,and the LOD was 8.8 μg·mL -1 .The precisions was 1.9%.The recovery of N,N dimethyl formamide was 101.4%.Three batches of sample were analysed.CONCLUSION After validation,the method was proved to be accurate,sensitive and reliable.It is quite suitable to be used in the analysis of the N,N dimethyl formamide in micronazed gilibenclamide capsules.