小儿感冒颗粒中香芹酮检查方法研究

Study on the Test Method of Carvone in Xiaoer Ganmao Granules

目的建立小儿感冒颗粒处方中薄荷药材可能掺有杂质留兰香(特征性成分香芹酮)的检测方法。方法采用气相色谱法(GC法)对小儿感冒颗粒中的香芹酮进行定性定量测定。样品采用乙酸乙酯提取,经毛细管柱(HP-5,30 m×0.32 mm×0.5μm)分离,氢火焰离子化检测器测定。外标法用于定量分析,气相色谱-串联质谱法(GC-MS/MS)用于对阳性样品进行确证。结果香芹酮的测定范围在1.07~42.82μg/mL,呈现良好的线性关系r=0.9992,平均回收率为97.57%,RSD为2.29%,检出限为1μg/g。结论所建立的方法准确可靠,操作简单,可用于小儿感冒颗粒中掺杂留兰香的定性及定量检查。

Objective In order to establish a detection method for the presence of impurities of spearmint(the characteristic ingredient carvone)in peppermint herbs used in the formulation of xiaoer ganmao granules.Methods Gas chromatography(GC)was used for qualitative and quantitative determination of carvone in xiaoer ganmao granules.The sample was extracted with ethyl acetate,separated by a capillary column(HP-5,30 m×0.32 mm×0.5μm),and detected by a hydrogen flame ionization detector.The external standard method was used for quantitative analysis,and the chromatography-tandem mass spectrometry(GC-MS/MS)was used for confirmation of positive samples.Results The determination range of carvone was 1.07-42.82μg/mL,exhibiting a good linearity linear relationship(r=0.9992),the average recovery rate was 97.57%,with an RSD of 2.29%,and the detection limit was 1μg/g.Conclusion The established method is accurate,reliable and easy to operate,and it can be applied to qualitative and quantitative analysis for impurities of carvone in xiaoer ganmao granules.