正红花油中血竭掺伪龙血竭检查方法的研究  

Research on the detection method of Draconis Sanguis adulterated Resina Draconis in Zhenghonghua oil

作　　者：刘岩庭 陈在敏 王勇 LIU Yan-ting;CHEN Zai-min;WANG Yong(Fujian Institute for Food and Drug Quality Control,Fuzhou 350012,China)

机构地区：[1]福建省食品药品质量检验研究院,福州350012

出　　处：《药物分析杂志》2024年第4期620-627,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：福建省科技计划项目(2020Y0073);国家药典委员会标准提高项目(2020Z007)。

摘　　要：目的:建立正红花油中血竭掺伪的检测方法。方法:以7,4’-二羟基黄酮为指标建立薄层色谱(TLC)法,快速筛查正红花油中掺伪的龙血竭。TLC筛查出可疑样品,用超高效液相色谱串联质谱(UPLC-MS/MS)法进行确证并定量分析,采用SuperLu C18(2)(100 mm×2.1 mm,1.8μm)色谱柱,以乙腈-水(25∶75)为流动相,流速0.3 mL·min^(-1),柱温25℃,选择m/z 253.1→117.1(定量)和m/z 253.1→91.0(定性)作为7,4’-二羟基黄酮检测离子对。结果:TLC方法专属性、耐用性良好。采用UPLC-MS/MS法,7,4’-二羟基黄酮质量浓度在0.470~37.58 ng·mL-1范围内线性良好(r=0.9997),加样平均回收率(n=6)为96.1%,RSD为3.2%。对30批正红花油进行薄层初筛,结果有24批疑似检出7,4’-二羟基黄酮。疑似样品通过UPLC-MS/MS验证,有24批正红花油超出拟定的限度,验证结果与TLC方法一致。结论:本方法快速,结果准确,灵敏度高,可用于正红花油中掺伪龙血竭筛查与分析。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,1.8μm),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=0.9997)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.

关 键 词：正红花油 7 4’-二羟基黄酮 掺伪 血竭 龙血竭 薄层色谱法 超高效液相-质谱联用 

分 类 号：R917[医药卫生—药物分析学]