染色沉香中10种非法染色剂检查方法的建立

Establishment of Inspection Method for Ten Illegal Dyes in the Dyed Aquilariae Lignum Resinatum

目的建立染色沉香中非法染色剂橙黄G、橙黄I、甲基橙、甲基黄、碱性橙21、金胺O、亮黄、柠檬黄、日落黄、皂黄的检查方法。方法采用薄层色谱(TLC)法对46批样品中上述10种非法染色剂进行筛查;采用超高效液相色谱-二极管阵列检测器(UPLC-DAD)法进行验证,色谱柱为Waters Acquity UPLC®BEH C_(18)柱(100 mm×2.1 mm,1.7μm),流动相为甲醇-0.2 mol/L乙酸铵溶液(梯度洗脱),检测波长为420 nm;采用高效液相色谱串联质谱(HPLC-MS/MS)法进行确认,离子源为电喷雾离子源,正负离子扫描模式。结果筛查出5批疑似检出柠檬黄、日落黄的样品;样品中被检成分与对照品保留时间一致,且图谱也一致;样品中相关物质的离子峰及碎片特征与2种对照品一致。结论所建立的方法可用于沉香中这10种非法染色剂的检查。

Objective To establish a method for the inspection of illegal dyes(orange G,orange I,methyl orange,methyl yellow,basic orange 21,auramine O,brilliant yellow,lemon yellow,sunset yellow and metanil yellow)in the dyed Aquilariae Lignum Resinatum.Methods Thin-layer chromatography(TLC)method was used to screen the above 10 illegal dyes in 46 batches of samples.Ultra-high performance liquid chromatography-diode array detector(UPLC-DAD)method was used for verification,and the chromatographic column was Waters Acquity UPLC®BEH C_(18) column(100 mm×2.1 mm,1.7μm),the mobile phase was methanol-0.2 mol/L ammonium acetate solution(gradient elution),and the detection wavelength was 420 nm.High-performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was used to confirm.Electrospray ion(ESI)was adopted as the ion source with positive and negative ion scanning mode.Results Five batches of suspected lemon yellow and sunset yellow samples were screened.The retention time and the UV spectra of the tested components in the test solution were consistent with those of the reference solution.The characteristics of related material ion peaks and fragments of the the test solution were consistent with those of two kinds of reference solution.Conclusion The established method can be used for the inspection of these ten illegal dyes in the dyed Aquilariae Lignum Resinatum.