目的:建立中药材蒲黄、黄柏和石斛中可能存在的染色剂金胺O的检测方法及阳性样品中金胺O的定量测定方法.方法:采用HPLC-MS/MS二级质谱对中药材蒲黄、黄柏和石斛中含金胺O的阳性样品进行定量测定,并进行方法学验证.质谱采用电喷雾正离子扫描(ESI+),二级质谱全扫描模式(production ion mode),母离子m/z 268.1,子离子扫描范围m/z 100～280.C18色谱柱(100mm×2.1 mm,1.9μm),柱温40℃,以2％磷酸溶液-乙腈为流动相,梯度洗脱,流速0.3 mL·min-1,进样量5μL,外标定量.结果:金胺O在0.776～7.760μg质量范围内与峰面积呈良好的线性关系(r=0.99991),平均回收率为100.9％(RSD=1.4％).结论:本方法具有良好的精密度、重现性和稳定性,线性关系良好,可用于中药材蒲黄、黄柏和石斛中金胺O的检测.
Determination of auramine O in pollen typhae,golden cypress and dendrobe by HPLC-MS/MS method
Objective:To develop a method for detecting,screening and quantifying the possibly exiting auramine O in Chinese patent medicines.Methods:HPLC-MS/MS was used for quantitative determination of auramine O in pollen typhae、golden cypress and dendrobe with ESI+ ion source. The ion at m/z 268.1 was selected as the precursor ion for MS/MS analysis and the resulting product ion spectrum was recorded between m/z 100 and m/z 280.C18 column (100 mm × 2.1 mm,1.9μm),the column temperature was maintained at 40 ℃, with 2％ phosphoric acid (A ) and acetonitrile(B)as mobile phase,gradient elution.The flow rate was 0.3 mL·min-1 ,the injection volume was 5μL ,quantitative.Results:There was a good linear relationship (r=0.99991)between the range and peak area,and the average recovery was 100.9％ (RSD=1.4％).Conclusion:This method is accurate and reliable,and can be used as the detection method for auramine O in pollen typhae、golden cypress and dendrobe.
Chinese medicinal materialsauramine OHPLC-MS/MSmethod study
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