嘧霉胺中有关物质的气相色谱-质谱分析

GC - MS Spectrum Analysis of Related Substances of Pyrimethanil

目的:用气相色谱-质谱法对嘧霉胺中的有关物质进行定性、定量分析。方法:采用GC-MS法对嘧霉胺的有关物质进行初步研究。气相色谱条件,色谱柱:HP-5MS 0.25 mm×30 m×0.25 μm,载气:高纯氦气,进样日温度:250℃,流量:1 mL·min-1,柱温:60℃以20℃·min-1速率升温至160℃保持1 min,再以30℃·min-1速率升温至280℃保持3 min,质谱条件,70 eV,EI电离源,扫描质量数30-300 amu。结果:得到了样品总离子流图及各相应的质谱图,对其进行解析,初步鉴定出嘧霉胺中的主要有关物质为A、B、C、D、E、F。结论:为研究嘧霉胺中有关物质来源用药安全和提高产品质量提供了科学依据。

Objective:To identify and quantify the related substances of pyrimethanil. Method: Analysis of the related substances of pyrimethanil was carried out by gas chromatography(GC) -mass spectrum (MS). The GC conditions were as follows:HP -5MS(30 m×0. 25 m ×0. 25 μm)capillary column,high purity helium was used as carrier gas,and the flow rate was 1. 0 mL· min-1 .injector temperature:250℃.column temperature:from 60℃ to 160℃ at rising rate of 20 ℃·min-1,keeping 160℃ 1 min,then from 160℃ to 280℃ at rising rate of 30℃·min-1,keeping 280· 3 min. The spectrometer was Agilent GC - MS 6890/5973N with electronic ionization(EI). Result:The total ion current and each chromatographic peck of select ion current were obtained,and resolution ofthese mass spectra was elucidated,the related substance A,B,C,D,E and F in pyrimethanil were identified. Conclusion : Scientific data are offered for studying whence of the related substance of pyrimetanil and improving its quality.