摘要
目的:建立通过超高效液相色谱-串联质谱法(UPLC-MS/MS),对川楝子药材中的川楝素进行定性鉴别及含量测定的方法。方法:样品经过甲醇加热回流提取后,采用UPLC-MS/MS,以乙腈-0.01%甲酸(31∶69)为流动相,以SB-C18色谱柱为分析柱,离子源为电喷雾电离负离子模式,分别采用Q3及Q1扫描模式,对川楝子中的川楝素进行快速定性定量检测。结果:所建立的方法能快速定性、定量检测川楝素,定性检测的离子对为m/z573.0→457.2,川楝素浓度在0.522~26.100μg/mL范围内线性良好,平均加样回收率为97.5%,检出限为6μg/g,定量限为20μg/g。结论:所建方法快速、准确、灵敏,适用于川楝子中川楝素的定性鉴别及含量测定。
Objective:To develop a UPLC-MS/MS method for qualitative and quantitative analysis of toosendanin in Fructus toosendan.Methods:Samples were heated with methanol under reflux and further detected by the ultra performance liquid chromatography-electrospray ion(ESI-)trap mass spectrometry method.The separation was performed with a isocratic elution(acetonitrile:0.01%formic acid=31∶69)using SB-C18 column.The qualitative and quantitative analysis of toosendanin was conducted in the Q1 and Q3 scan mode.Results:The m/z 573.0→457.2 was two qualitative ion pair of toosendanin.The calibration curves showed good linear relationship in the range of 0.522~26.100μg/mL for the component.The detection limit was 6μg/g,the quantization limit was 20μg/g,and the average recovery rate was 97.5%.Conclusion:The method was proved to be rapid,accurate and sensitive,which can be used to qualitative and quantitative analysis of toosendanin in Fructus toosendan.
作者
梁镇然
吴愫青
Liang Zhenran;Wu Suqing(Zhuhai Institute for Food and Drug Control,Zhuhai 519000,China)
出处
《广东化工》
CAS
2023年第20期155-156,175,共3页
Guangdong Chemical Industry
