建立了超高效液相色谱-串联质谱检测枳实药材中辛弗林、N-甲基酪胺的方法.以甲醇为提取溶剂,经QuECHERS分散净化,采用资生堂CAPCELL PAK CR色谱柱(150 mm×2.0 mm,5 μm;C18和SCX比例为1∶4)分离,质谱以正离子扫描,反应监测模式测定.辛弗林和N-甲基酪胺在10～2 000 ng/mL范围内线性关系良好(R2＞0.997),检出限和定量限分别为0.3 ng/mL和1.0 ng/mL,回收率范围为94.3％～105.7％,相对标准偏差(RSD)均小于3％.该方法避免了使用磷酸盐和离子对试剂,仅在流动相中添加甲酸和甲酸铵,分析物就能有较好的保留,具有极高的质谱响应.相较于传统方法,该方法分析时间短、操作简单、专属性强,在强极性生物碱分离检测方面具有较好的应用价值.
Determination of Synephrine and N-Methyl Tyramine in Frutus Aurantii Immaturus by QuECHERS with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
An ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)method for the determination of synephrine and n-methyl tyramine in Frutus Aurantii Immaturus was established.The samples were extracted with methanol,and purified by QuECHERS.The separation was performed on Shiseido CAPCELL PAK CR column(2.0 mm ×150 mm,5 μm;C18 to SCX ratio of 1∶4),and the samples were determined by positive ion scanning with multi-reaction monitoring mode.The linear relationship of synephrine and n-methyl tyramine was good in the range of 10-2 000 ng/mL(R2＞0.997).The limit of detection(LOD)and limit of quantification(LOQ)of synephrine and n-methyl tyramine were 0.3 ng/mL and 1 ng/mL,respectively.The recovery range was 94.3％-105.7％,and relative standard deviations(RSDs)were all less than 3％.This method avoids using phosphate and ion pair reagents,and only adding formic acid and ammonium formate in the mobile phase.The analytes have good retention and very high mass spectral response.Compared with the traditional method,this analytical method is fast,simple,specific,and it has a good application value in the separation and detection of large polar alkaloids.
UPLC-MS/MSIon exchange and C18 hybrid columnSynephrineN-Methyl tyramineQuECHERS
万方数据
维普
