Determination of ten illegal dyes in Gejie Dingchuan Pills
LUO Yi1 QIU Mingming1 HE Songhua1 LIN Jingkai1 WU Yuqiang2▲
1.Guangxi Institute for Food and Drug Control, Guangxi Zhuang Autonomous Region, Nanning 530021, China;
2.Pharmaceutical Factory of Guangxi Traditional Chinese Medical University, Guangxi Zhuang Autonomous Region, Nanning 530023, China
Abstract：Objective To establish a quantification method of HPLC for determining illegally added auramine O, lemon yellow, carmine, sunset yellow, brilliant yellow, acid red, methyl orange, orange Ⅱ, etythrosine and alkaline orange in Gejie Dingchuan Pills, and validate with LC-MS/MS method. Methods The sample was extracted by 50% ethanol, and determined by HPLC with a gradient elution of acetonitrile-0.01 mol/L ammonium acetate (contain 0.5% glacial acetic acid) and the detection wavelength was set at 420 nm and 500 nm. The identification was performed by LC-MS/MS, using a gradient elution of acetonitrile-0.01 mol/L ammonium acetate. The analytes were detected by an electro spray ionization tandem mass spectrometry with dynamic MRM. Qualitation of the auramine O based on the retention time and mass charge ratio. Results The calibration curve of ten dyes showed good linearity and correlation coefficients were all above 0.999, the limits of quantitation for ten dyes in samples were between 0.3-2.8 μg/g, and the average recoveries ranged from 96.3% to 101.1% with RSD of 0.6%-1.5%. Auramine O could be detected in 33 of 123 samples. Conclusion LC-MS/MS method is accurate and reliable for the qualitative identification and the HPLC method is simple, rapid and accurate for the content determination. The combination of HPLC and LC-MS/MS can detect ten dyes in Gejie Dingchuan Pills rapidly, accurately and sensitively.
2017, Vol. 14 
京公网安备 11010502046598号