高效液相色谱-串联质谱法测定龙血碣药材中苏丹红Ⅳ  

Determination of sudanⅣin resina draconis crude drug by high performance liquid chromatography-tandem mass spectrometry

作　　者：李柯 杨蕾[1] 孟令嘉 Li Ke;Yang Lei;Meng Lingjia(Beijing Shijitan Hospital affiliated to Capital Medical University,Beijing 100038,China)

机构地区：[1]首都医科大学附属北京世纪坛医院,北京100038

出　　处：《化学分析计量》2021年第11期37-41,共5页Chemical Analysis And Meterage

摘　　要：建立高效液相色谱串联质谱法测定龙血碣药材中苏丹红Ⅳ染色剂的方法。样品经乙腈提取后,采用Agilent-C_(18) XDB色谱柱(250 mm×4.6mm,5μm)进行分离,流动相为乙腈-0.02%甲酸水(体积比为95∶5),流量为1.0 mL/min,柱温为30℃,进样体积为10μL,检测波长为518 nm。质谱条件:ESI离子源,正离子模式扫描,液氮为干燥气和雾化器,流量为3.0 mL/min,加热气为空气,流量为10.0 mL/min,采用多反应监测(MRM)模式进行定量分析。苏丹红Ⅳ的浓度在1.142~141.0μg/mL范围内与色谱峰面积具有良好的线性关系,相关系数为0.9999。样品加标回收率为94.72%~99.21%,6次重复测定结果的相对标准偏差为1.12%。该方法操作简单、准确,可以用于龙血碣药材中非法染色苏丹红Ⅳ的含量测定,同时为保证龙血碣药材的安全用药提供实验参考。A method for determination of sudanⅣin resina draconis crude drug by high performance liquid chromatography-tandem mass spectrometry was established.The samples were extracted with acetonitrile aqueous solution and the Agilent-C_(18) chromatography column(250 mm×4.6 mm,5μm)was performed to separation with acetonitrile-0.02%formic acid(Volume ratio was 95∶5)as the mobile phase at the flow rate of 1.0 mL/min,the detection wavelength was 518 nm,the column temperature was maintained at 30℃and the injection of volume was 10μL.Multiple response monitoring model was used to qualitative analysis with ESI ion source and positive ion scanning,liquid nitrogen was used as dry gas and nebulizer gas with the flow rate of 3.0 mL/min,the heater gas was air with the flow rate of 10.0 mL/min.The concentration of sudanⅣexhibited good linearity with the chromatographic peak area among the ranges of 1.142-141.0μg/mL,the coefficient of correlation was 0.9999.The recovery was 94.72%-99.21%,the relative standard deviation of 6 determination results was 1.12%.The method is simple and accurate which can be used for determination of SudanⅣin resina draconis crude drug.At the same time.the method can provide experiment reference and ensure the safety for the clinical use.

关 键 词：龙血碣 非法染色剂 苏丹红Ⅳ 液相色谱串联质谱 

分 类 号：O657.7[理学—分析化学]