液相色谱-串联质谱法测定茶叶中二氰蒽醌残留量

Determination of dicyanoanthaquinone residues in tea using liquid chromatography tandem mass spectrometry

中文关键词:  液相色谱串联质谱仪  二氰蒽醌  茶叶

英文关键词:liquid chromatography tandem mass spectrometry  dicyanoanthraquinone  tea

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography tandem mass spectrometry, LC-MS/MS)测定茶叶中二氰蒽醌残留。方法 茶叶用乙腈(含0.1%甲酸)提取, 经固相萃取柱(HC-C18 SPE)净化后采用多反应监测(multiple reaction monitoring, MRM)模式进行检测, 外标法定量。结果 目标化合物在一定范围内(0.391~12.5 μg/L)线性关系良好, 相关系数(r2)大于0.995。样品中二氰蒽醌的定量限(limit of quantification, LOQ)和检出限(limit of detection, LOD)分别为10.0、5.00 μg/kg; 不同加标浓度样品10.0 μg/kg(LOQ)、20.0 μg/kg (2×LOQ)、50.0 μg/kg(5×LOQ)的平均回收率为84.1%~103%, 相对标准偏差(RSDs)为3.18%~4.62%。25份市售茶叶中均未检出二氰蒽醌。结论 该方法简便、快速, 准确。各项性能参数均能符合技术规范的要求, 已应用于市售茶叶的检测。

英文摘要:

      Objective To establish a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the determination of dicyanoanthraquinone residues in tea. Methods Dicyanoanthraquinone residue in tea was extracted with acetonitrile (containing 0.1% formic acid). After purification with HC-C18 solid-phase extraction column, the analyte was tested by LC-MS/MS in multi-reaction monitoring model and quantified by external standard method. Results The linear relationship of the target compound was good in a certain range (0.391–12.5 μg/L), and the correlation coefficient (r2) was greater than 0.995. The limit of quantification (LOQ) and limit of detection (LOD) of dicyanoanthraquinone in the sample were 10.0 and 5.00 μg/kg respectively. The average recoveries of 10.0 μg/kg (LOQ), 20.0 μg/kg (2×LOQ) and 50.0 μg/kg (5×LOQ) were 84.1%–103%, and the relative standard deviations (RSDs) were 3.18%–4.62%. Dicyanoanthraquinone was not detected in 25 commercial tea leaves. Conclusion The method is simple, rapid and accurate. All the performance parameters can meet the requirements of the technical specifications, and the method has been applied to the detection of commercial tea.