HPLC-DAD-MS/MS法结合谱库筛查5种中药中21种合成染料  

Screening of twenty-one synthetic dyes in five kinds of traditional Chinese medicines by HPLC-DAD-MS/MS combined with spectrum library

作　　者：何轶[1] 雷银瓶 鲁静[1] 王瑞忠[1,3] 何风艳[1] 戴忠[1] 马双成[1] 

机构地区：[1]中国食品药品检定研究院,北京100050 [2]中国医学科学院药物研究所,北京100050 [3]山西中医学院,山西太原030024

出　　处：《中成药》2016年第12期2631-2635,共5页Chinese Traditional Patent Medicine

基　　金：公益性行业科研专项资助项目(2012104008-1)

摘　　要：目的通过高效液相色谱-二极管阵列检测-串联质谱（HPLC-DAD-MS/MS）法结合谱库筛查龙血竭、红花、跌打丸、二十五味珊瑚丸、跌打活血散中21种合成染料（金胺O、金橙Ⅱ、胭脂红等）。方法 7批阳性样品甲醇或乙醇提取液的分析采用Phenomenon Luna C18色谱柱（250 mm×4.6 mm,5μm）;以乙腈-0.05 mol/L醋酸铵为流动相,梯度洗脱;体积流量1 m L/min;柱温40℃;检测波长400~700 nm。MS分析采用ESI电离源;干燥气温度350℃,体积流量10 L/min;雾化气压力241.3 k Pa;源电压4 k V。结果所有样品均检测出合成染料,谱库匹配度均大于99.8。结论该方法准确快速,可用于中药中合成染料筛查。AIM To screen twenty-one synthetic dyes（ auramine O,orange Ⅱ,carmine,etc.） in Resina Draconis,Carthami Flos,Dieda Pills,Ershiwuweishanhu Pills and Diedahuoxue Powder by high performance liquid chromatography-diode array detector-tandem mass spectrometry（ HPLC-DAD-MS / MS） combined with spectrum library. METHODS The analyses of methanol or ethanol extracts of seven batches of positive samples were per-formed on a 40 ℃ thermostatic Phenomenex Luna C18column（ 250 mm × 4. 6 mm,5 μm）,with the mobile phase comprising of acetonitrile-0. 05 mol / L ammonium acetate at a flow rate of 1 mL / min in a gradient elution manner,and the detection wavelengths were set at 400- 700 nm. Electrospray ion（ ESI） source was adopted in the MS analysis,the gas temperature was maintained at 350 ℃ flowing at 10 L / min,the nebulizer pressure was 241. 3 kP a,and the source voltage was 4 k V. RESULTS The synthetic dyes were detected in all the samples,whose matching degrees of spectrum library were all more than 99. 8. CONCLUSION This accurate method can be used for the rapid screening of synthetic dyes in traditional Chinese medicines.

关 键 词：中药 合成染料 HPLC-DAD-MS/MS 谱库 

分 类 号：R284.1[医药卫生—中药学]