气相色谱–串联质谱法快速测定茶叶中的蒽醌

建立气相色谱–串联质谱法(GC–MS–MS)快速测定茶叶中蒽醌的方法。样品中的蒽醌用色谱纯乙腈提取,经过涡旋1 min,超声20 min,离心、浓缩后用固相萃取柱(SPE)净化,以DB–5MS毛细管柱分离,以m/z 207.9,152为定性离子对、m/z 207.9,180为定量离子对,多反应检测模式下测定,外标法定量。蒽醌的质量浓度在1~500μg/L范围内与定量离子的峰面积呈良好的线性关系,相关系数为0.999 98,方法的检出限为1μg/kg。在10,20,50μg/kg加标水平下,样品加标回收率为92.85%~98.10%,测定结果的相对标准偏差为8.50%~11.05%(n=5)。该方法简单、快速,检出限低,准确度和精密度高,可用于茶叶中蒽醌的检测。

Determination of Anthraquinone in Tea by GC-MS-MS

The method for determination of anthraquinone in tea by gas chromatography-tandem mass spectrometry(GC-MS-MS) was established. The sample was extracted by acetonitrile of chromatographic purity, vortexed for 1 min, sonicated for 20 min, centrifuged and concentrated, then the extracts were purified by solid phase extraction(SPE). After being separated on DB-5MS capillary column, the target analyte was detected by GC-MS-MS under the multi reaction monitoring mode with a qualitative ion pair (m/z 207.9, 152) and a quantitative ion pair (m/z 207.9, 180), and quantified by the external standard method. The anthraquinone concentration and peak area of quantification ion had good relationship in the range of 1-500 μg/L, the correlation coefficient was 0.99998. The detection limit was 1 μg/kg. The recoveries for 10, 20, 50 μg/kg spiked levels ranged from 92.85％ to 98.10％, and the relative standard deviation of determination results was 8.50 ％-11.05％(n=5). The method is suitable for determination of anthraquinone in tea with advantages of simple and rapid sample processing, low detection limit, high accuracy and precision.