马蔺子素中残留乙醇、乙酸乙酯的测定

目的应用顶空气相色谱法,对马蔺子素中的残留溶剂乙醇和乙酸乙酯进行测定。方法采用固定相为94%二甲基聚硅氧烷-6%氰丙基苯基,0.53mm×30m,膜厚3.0μm的色谱柱,以氮气为载气,FID检测器,通过外标法计算残留溶剂的含量。结果马蔺子素中有乙醇检出,乙酸乙酯未检出。乙酸乙酯的线性范围:2.22～666μg(r=0.9999);乙醇的线性范围:4.84～484μg(r=0.9998);定量限乙醇为4.8ppm,乙酸乙酯为2.2ppm;检测限乙醇为0.5ppm,乙酸乙酯为0.4ppm。平均回收率乙醇为105.2%,乙酸乙酯为95.2%。结论本方法简便、灵敏度高、重复性好,结果准确。

Determination of ethanol and ethyl acetate remained in Irisquinone

Objective A gas chromatograph with a headspace sampler was used to determine ethanol and ethyl acetate of Irisquinone.Methods The solid phase is 6%cyanopropylphenyl-94%dimethylpolysiloxane,0.53mm×30m,thickness is 3.0μm,carrier gas is N_2,detector is FID,ISTD method is used to determine the assay.Results In the sample of Irisquinone,the ethanol is detected and ethyl acetate is not detected.The linearity range of ethyl acetate is 2.22～666μg(r=0.9999).The linearity range of ethanol is 4.84～484μg(r=0.9998),the LOQ of ethanol is 4.8ppm,the LOQ of ethyl acetate is 2.2ppm;the LOD of ethanol is 0.5ppm,the LOD of ethyl acetate is 0.4ppm,the average recovery of ethanol is 105.2%,that of ethyl acetate is 95.2%.Conclusion The method is simple,sensitive,exactive and has good repeatability.