红花中非法添加色素的薄层色谱快速鉴别法

Rapid TLC Identification Method of Illegally Added Pignent in Carthami Flos

目的:针对各省药品质量公告中红花中非法添加色素的报道,按现行国家补充检验批件仅能检出色素金橙Ⅱ,现建立快速薄层色谱方法,以补充检验红花药材中可能含有的除金橙Ⅱ外其他类非法添加的色素。方法:采用薄层色谱法,硅胶G为固定相,70%乙醇为溶剂,乙酸乙酯-正丁醇-乙醇-氨水-水(1∶3∶3∶1∶1)为展开剂,在可见光下检视筛查;采用高效液相色谱法(HPLC),以十八烷基硅烷键合硅胶为填充剂,甲醇-0.05 mol·L-1醋酸铵(52∶48)为流动相,柱温35℃,检测波长508nm,用紫外检测器和二极管阵列检测器进行两次检测,通过与对照试剂色谱峰比对进一步加以确证。结果:在薄层色谱和HPLC佐证结果一致情况下,抽查的9批红花药材中确证有两批药材含食品禁用色素酸性红73。结论:该薄层方法简单、快速、重复性好,成本低,适用于药品检测车的快速筛查红花中非法添加色素,补充了红花国家标准中的相关规定,对进一步加大对中药材、中药饮片市场的监管,对开展染色掺假中药专项整治具有较强的实用性。

Objective：This article was aimed to establish a rapid identification method for the detection of illegally added pigments in Carthami Flos besides golden orange pigment Ⅱ in the case of that only golden orange pigment Ⅱ can be detected according to the current national inspection approval of to supplement the inspection of illegally added pigment in Carthami Flos besides golden orange pigment Ⅱ.Method：In TLC method,silicagelG was used as stationary phase,70％ ethanol was used as solvent,and ethylacetate-butanol-ethanol-ammonia-water （1∶3∶3∶1∶1） was used as developing solvent,and the result was detected under visible light.The positive samples were further proved by HPLC method.In HPLC method,octadecylsilane bonded silica was used as a filler,methanol-0.05 mol·L-1 ammonium acetate （52∶48） was used as mobile phase.The column temperature was 35 ℃,the detection wavelength was 508 nm,by tested twice with ultraviolet detector and photodiode array detector.Then the result was compared with the peak of the control reagents for further confirmation.Result：The results of two positive samples by TLC were consistent with those by HPLC.Two out of nine groups of Carthami Flos samples were proven to contain the forbidden food pigment acid red 73.Conclusion：The method is suitable for rapid screening of illegally added pigment in Carthami Flos.The established TLC method is simple,rapid,reproducible,cost-effective,to supplement the relevant provisions of national standards,and to play a significant role in the management of medicine timber and Chinese Herbal Medicine.