HPLC-MS法检测少腹逐瘀丸及原料药材中非法添加的7种黄色素  

Determination of seven yellow pigments illegally added into Chinese materia medica by HPLC-MS

作　　者：连云岚 杜娟 乔玉峰 

机构地区：[1]山西省食品药品检验所,山西太原030001 [2]山西振东制药股份有限公司,山西长治047100

出　　处：《中草药》2016年第18期3219-3223,共5页Chinese Traditional and Herbal Drugs

摘　　要：目的建立一种用于快速检测中药中非法添加的7种黄色素（柠檬黄、日落黄、灿烂黄、金橙II、金胺O、碱性橙21、碱性橙）的HPLC-MS方法。方法样品采用70%乙醇溶液超声提取,以反相C18为色谱柱分离,以乙腈-0.05 mol/L醋酸铵水溶液为流动相梯度洗脱,HPLC以二极管阵列检测器在432 nm处检测,质谱检测器选择ESI离子源、正离子扫描检测。结果在上述色谱及质谱条件下,7种常用黄色系色素分离度、专属性及耐用性良好,精密度RSD在0.4%~1.8%;色素溶液在24 h内稳定,RSD〈1.9%;准确度试验回收率在95.1%~102.9%;检出限（LOD）在2~31μg/kg;重复性RSD在0.3%~1.4%。3批次市售中药中均检出金胺O。结论方法简便、快速、重复性好、灵敏度高,可用于检测易染色中药中非法添加的7种黄色素,为有关企业或食品药品监督管理部门控制中药质量提供一定的参考。Objective To establish a rapid method for the simultaneous determination of seven yellow pigments（tartrazine, sunset yellow, brilliant yellow, orange II, auramine O, astrazon orange G, and basic orange） which were illegally added into Chinese materia medica（CMM）. Methods The sample was extracted with ultrasonic by 70% ethanol, separated on a reversed phase C18 chromatographic column by gradient elution using a mobile phase made up of acetonitrile and 0.05 mol/L ammonium acetate solution, and then detected by diode array detector in the wavelength of 432 nm and mass spectrometry detector with ESI＋ ion source. Results Under the condition of the above chromatography and mass spectrometry, the separating degree, specificity, and durability of the seven yellow pigments were good. RSD of precision was between 0.4%—1.8%. Above pigment solution was stable in 24 h and RSD 1.9%. The recovery rates of accuracy were between 95.1%—102.9%. The limits of detection（LODs） were in the range of 2—31 μg/kg, and the RSD of repeatability was in the range of 0.3%—1.4%. Auramine O was detected in three batchs of CMM for sale. Conclusion This method is simple, rapid, reproducible and has high sensitivity, which can be used for the determination of seven yellow pigments illegally added into dyed CMM, and it can provide the reference or help for relative company and State Food and Drug Administration in controlling the quality of CMM.

关 键 词：中药 非法染色 HPLC-MS 蒲黄 延胡索 柠檬黄 日落黄 灿烂黄 金橙Ⅱ 金胺O 碱性橙21 碱性橙 

分 类 号：R286.02[医药卫生—中药学] R917[医药卫生—中医学]