气相色谱-质谱法测定当归粉、当归原药材中的邻苯二甲酸二丁酯

摘要

A simple method for the determination of dibutyl phthalate (DBP) in Angelica sinensis and its powder by gas chromatography-mass spectrometry was established. On the basis of GB standards, the single-factor experiment was employed to optimize the extraction method and the solvent. Hexane as the extractant was determined and the method of liquid-liquid extraction from water was established. The methodological study showed that r2 of linear regression was 0.999 5 in the range of 0.01-1.00 μg/mL DBP, TIC limit of the detection was 0.05 μg/g, the recoveries at different levels ranged from 90% to 100% with relative standard deviations less than 5%(n=3). The method can meet the requirements of daily analysis of DBP in angelica sinensis and its powder.%建立了气相色谱-质谱法测定当归粉和当归原药材中邻苯二甲酸二丁酯( DBP)的方法.在国家标准的基础上,通过单因素试验,优化了提取方法和提取溶剂,确定了以正己烷为提取剂从水中液液萃取的方法.方法学试验结果表明,DBP浓度在0.01～1.00 μg/mL范围内与色谱峰面积呈良好的线性关系,线性相关系数r2=0.9995,检出限为0.05 μg/g(全扫描),不同水平的加标回收率在90％～100％之间,测定结果的相对标准偏差小于5％(n=3).该方法适合当归粉和当归原药材中DBP的日常检测.