液相色谱-串联质谱法同时测定蒲黄、黄柏和石斛中的金胺O  

Determination of auramine O in pollen typhae,golden cypress and dendrobe by HPLC-MS/MS method

作　　者：裴春梅 杨洋 李英杰 史永惠 孟美英 丁华 Pei Chun-mei;Yang Yang;Li Ying-jie;Shi Yong-hui;Meng Mei-ying;Ding Hua(Ordos Inspection and Testing Center,Ordos 017010,China)

机构地区：[1]鄂尔多斯市检验检测中心,内蒙古鄂尔多斯017010

出　　处：《北方药学》2024年第5期5-7,15,共4页Journal of North Pharmacy

摘　　要：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。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,1.9 μm),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.

关 键 词：中药材 金胺O 液相色谱-质谱联用 方法研究 

分 类 号：R927[医药卫生—药学]