摘要
目的:建立以薄层色谱为初筛,高效液相色谱验证相结合的方法,以补充检验朱砂药材中非法添加颜料红531、颜料红571、酸性红73、偶氮玉红、胭脂红5种色素。方法:采用薄层色谱法,硅胶G为固定相,70%乙醇为溶剂,正丁醇-乙醇-冰乙酸-水(8∶4∶2∶2)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,流动相为乙腈-0.02 mol·L-1醋酸铵梯度洗脱,柱温30℃,检测波长237 nm,用二极管阵列检测器进行检测,通过与颜料红531、颜料红571、酸性红73、偶氮玉红、胭脂红对照试剂色谱峰比对加以确证,以液质联用对结果加以验证。结果:在薄层色谱和HPLC验证结果一致情况下,68批朱砂样品中,有8批样品分别含有上述1种或几种色素添加。结论:该方法简单、快速、重复性好、成本低,补充了朱砂饮片国家药品标准中的相关规定,对进一步加大对中药材中药饮片市场的监管以及开展染色掺假中药专项整治具有较强的实用性。
Objective： To establish an identification method using TLC as preliminary screen and HPLC as verification to supplement the detection of 5 illegally added pigments, such as Pigment Red 531, Pigment Red 571, Brilliant Crocein, Azorubine, Ponceau 4R in cinnabaris. Methods： In the TLC method, silica gel G was used as a stationary phase, 70% ethanol was used as the solvent, and butanol-ethanol-aceticacid-water （8 ： 4 ： 4 ： 2） was used as developing solvent, and the result was detected under visible light. In HPLC method, octadecylsilane bonded silica was used as a filler, acetonitrile-0.02 mol ~ L1 ammonium acetate was used as mobile phase. The column temperature was 30~C and the detection wavelength was 237 urn, photodiode array detector was used to do the detection. Then the result was compared with the peak of the control reagents of Pigment Red 531, Pigment Red 571, Brilliant Crocein, Azorubine, Ponceau 4R for confirmation. The results were further validated by the LC-MS, Results： The results of the TLC were consistent with those of HPLC. 8 out of 68 batches of cinnabaris samples were proven to contain the above-mentioned one or more pigments. Conclusion： The method is simple,rapid, reproducible, cost-effective and can supplement the relevant provisions of national standards for decoction pieces of cinnabaris, which is very practical in strengthening the supervision of Chinese herbal medicine market and in carrying out special rectification of dyeing and adulteration of traditional Chinese medicine.
作者
丁野
聂平
孙辉
席洋
胡亮
马杰
李文莉
魏锋
Ding Ye;Nie Ping;Sun Hui;Xi Yang;Hu Liang;Ma Jie;Li Wenli;Wei Feng(Hunan Institute for Drug Control,Changsha 410001,China;School of Pharmaceutical Sciences,Central South University,Changsha 410008,China;National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《中国药事》
CAS
2018年第10期1373-1381,共9页
Chinese Pharmaceutical Affairs
基金
十二五国家科技重大专项(编号2014ZX09304307-002)
2015年国家药品计划抽验项目
湖南省食品药品监督管理局食品药品安全科技项目(编号湘食药科R201707)
