Research on the detection method of Draconis Sanguis adulterated Resina Draconis in Zhenghonghua oil
Objective:To establish a screening method for the detection of adulteration of Draconis Sanguis in Zhenghonghua oil.Methods:To establish a thin layer chromatography(TLC)method with 7,4'-dihydroxyfla-vone as an index for fast screen of the adulteration in Zhenghonghua oil.The suspected samples were screened by TLC and the quantification was performed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The chromatographic column was SuperLu C18(2)(100 mm ×2.1 mm,1.8 μm),the mobile phase was acetonitrile-water(25∶75)at a flow rate of 0.3 mL·min-1 and the column temperature was 25 ℃.The detection ion pairs for 7,4'-dihydroxyflavone were m/z 253.1→117.1(quantitative)and m/z 253.1→91.0(qualitative).Results:TLC method was specific and durable.The linear range of 7,4'-dihydroxyflavone was 0.470-37.58 ng·mL-1(r=0.999 7)by UPLC-MS/MS.The average recovery rate(n=6)was 96.1％and RSD was 3.2％.Thirty batches of Zhenghonghua oil were screened by TLC,and 24 batches were suspected to have 7,4'-dihydroxyflavone.The suspected samples were verified by UPLC-MS/MS,24 batches of Zhenghong-hua oil exceeded the proposed limit,and the verification results were consistent with TLC method.Conclusion:This method is rapid,accurate and can be used for the screening and analysis of adulterated Zhenghonghua oil.
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