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应用气相色谱-质谱/质谱法测定了茶叶中蒽醌残留量。前处理方法包括添加同位素内标蒽醌-D8,正己烷-丙酮(1:1,V/V)提取,弗罗里硅土柱净化,正己烷-乙醚(8:2,V/V)洗脱。采用HP-5MS色谱柱(30 m×0.25 mm×0.25μm)并使用程序升温过程对样品进行分离。选择反应监测模式(SRM),蒽醌两对离子进行定性、定量分析,内标法定量。蒽醌在0~200!g/L范围内具有良好的线性关系,相关系数大于0.9990。在0.02,0.04和0.08 mg/kg 3个添加水平,绿茶、红茶、乌龙茶、普洱茶平均回收率范围为84.2%“98.1%,相对标准偏差小于9.7%,定量限为0.02 mg/kg。方法可用于茶叶样品中蒽醌残留的确证检测。
The anthraquinone residues in tea were determined by gas chromatography-mass spectrometry / mass spectrometry. The pretreatment methods included adding isotope internal standard anthraquinone-D8, extracting with n-hexane-acetone (1: 1, V / V), purifying with Florisil and purifying n-hexane- Off Samples were separated on a HP-5MS column (30 m × 0.25 mm × 0.25 μm) using a programmed temperature ramp. Select reaction monitoring mode (SRM), anthraquinone two pairs of ions qualitative and quantitative analysis, internal standard method. Anthraquinone has a good linear relationship in the range of 0 ~ 200 μg / L, the correlation coefficient is greater than 0.9990. The average recoveries of green tea, black tea, oolong tea and Pu’er tea were 84.2% ”98.1% with relative standard deviations less than 9.7% and the limit of quantification was 0.02 mg / kg at the three addition levels of 0.02, 0.04 and 0.08 mg / It can be used to confirm the detection of anthraquinone residues in tea samples.