气相色谱法测定格列本脲胶囊中二甲基甲酰胺的含量

摘　要：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100%二甲基聚硅氧烷为固定相，柱温150℃维持14min，以40℃^.min^-1的速率升温至200℃，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(0.088%)。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。

关键词：气相色谱法；格列本脲胶囊；二甲基甲酰胺

分类号：TQ460.7+2　文献标识码：A
文章编号：1001-2494(2001)02-0120-03

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

WANG Wei（Tianjin Institute for Durg Control,Tianjin 300070,China）　

Abstract：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.

Keywords：gas chromatography;micronazed gilibenclamide capsules;N,N-dimethyl formamide

参考文献：

［1］中国药典1990年版.药典注释[S]，1990：469.
［2］中国药典2000年版.二部[S].附录，2000：64.

收稿日期：2000年6月27日

出版日期：2001年2月8日