超高效液相色谱-串联四极杆-静电场轨道阱-线性离子阱质谱法测定中药中7种杂环胺类物质

Determination of seven heterocyclic aromatic amines in Chinese medicine by ultra performance liquid chromatography-quadrupole-orbitraplinear ion trap mass spectrometry

目的建超高效液相色谱-串联四极杆-静电场轨道阱-线性离子阱质谱法检测中药中7种杂环胺类物质的分析方法。方法以0.1%的甲酸水溶液和乙腈为流动相,采用Waters Acquity UPLC BEH C18反相色谱柱(100 mm×2.1 mm,1.7µm)梯度洗脱,流速为0.3 mL/min,在正离子模式下扫描,高分辨一级定量模式下测定。结果7种杂环胺类物质线性关系良好,相关系数大于0.957,检出限为0.02µg/L,在3个加标水平下,杂环胺类物质在焦山楂、焦麦芽、焦神曲和炒鸡内金4种中药中的平均回收率为72.1%~119.6%,相对标准偏差为0.6%~16.4%。结论该方法具有灵敏度高和准确性强等优点,适用于中药中杂环胺的精确检测。

Objective To establish an analytical method for the simultaneous determination of seven heterocyclic aromatic amines in Chinese medicine by ultra-high performance liquid chromatographyquadrupole-electrostatic field track trap-linear ion trap mass spectrometry.Methods The separation was achieved by Waters Acquity UPLC BEH C18 column(100 mm×2.1 mm,1.7µm)and a gradient elution with the mobile phases of acetonitrile and 0.1%formic acid.The flow rate was set at 0.3 mL/min.The target compound was scanned in the positive ion mode and analyzed in high-resolution quantitative mode.Results The linear relationship of the seven heterocyclic amines was good,and the correlation coefficients of the seven heterocyclic aromatic amines were all above 0.957 and the limits of detection were 0.02µg/L.The recoveries of the seven heterocyclic aromatic amines in all samples were 72.1%‒119.6%,the relative standard deviations were 0.6%‒16.4%.Conclusion This method has the advantages of high sensitivity and accuracy,and is suitable for the accurate detection of heterocyclic amines in traditional Chinese medicine.