论文部分内容阅读
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 an HPLC-MS method for the rapid determination of seven yellow pigments (lemon yellow, sunset yellow, brilliant yellow, golden orange II, aurine O, basic orange 21, and basic orange) illegally added to traditional Chinese medicine. Methods The samples were extracted with 70% ethanol solution by ultrasonic and separated by reversed-phase C18 column. The mobile phase was eluted with acetonitrile-0.05 mol / L ammonium acetate aqueous solution. HPLC was detected with a diode array detector at 432 nm. ESI source selected, positive ion scan detection. Results Under the above chromatographic and mass spectrometric conditions, the seven commonly used yellow pigments showed good resolution, specificity and durability with a RSD of 0.4% -1.8%. The pigmentation solution was stable within 24 h with RSD <1.9%. Accuracy The test recoveries ranged from 95.1% to 102.9%, the limits of detection (LOD) ranged from 2 to 31 μg / kg, and the repeatability RSD ranged from 0.3% to 1.4%. Three batches of commercially available Chinese medicine were detected gold amine O. Conclusion The method is simple, rapid, reproducible and sensitive. It can be used to detect the seven kinds of yellow pigments illegally added in easily-stained traditional Chinese medicines. It can provide reference for enterprises or food and drug administrations to control the quality of traditional Chinese medicine.