气相色谱-质谱联用法测定茶叶包装纸中9,10-蒽醌含量

Determination of 9,10-Anthraquinone in Tea Packaging Paper by GC-MS/MS

建立气相色谱-质谱联用(GC-MS-MS)检测茶叶包装纸中9, 10-蒽醌方法。样品采用丙酮-正己烷混合溶液提取,提取液经离心、氮吹浓缩后,过弗罗里硅土固相萃取柱SPE净化,净化液进入气质联用仪分析,仪器采用DB-5MS气相色谱柱(20 m×0.18 mm×0.18μm)分离,选择多反应监测模式扫描,内标法定量。结果表明,该方法在10~200 ng/mL质量浓度范围内具有良好的线性关系,线性回归方程为Y=0.23249X+0.001203,拟合度R^(2)为0.9989,方法检出限为3μg/kg,定量限为10μg/kg,加标回收率在89.3%~98.7%之间,相对标准偏差(RSD)为3.01%~4.42%。该方法适用于茶叶包装纸中9,10-蒽醌定性定量检测。

A gas chromatography-mass spectrometry(GC-MS-MS)method was established for the detection of 9,10-anthraquinone in tea packaging paper.The sample was extracted with acetone-n-hexane mixed solution,and then the extract was concentrated by centrifugation and nitrogen blowing,and then purified by SPE with a Florisil solid phase extraction column.The purified liquid was analyzed by a gas-mass spectrometer.The instrument used DB-5 MS gas chromatography.Column(20 m×0.18 mm×0.18μm)was separated,scanning in multi-reaction monitoring mode was selected,and internal standard method was used for quantification.The results showed that the method had a good linear relationship in the mass concentration range of 10~200 ng/mL,the linear regression equation was Y=0.23249 X+0.001203,the fit R^(2) was 0.9989,the detection limit of the method was 3μg/kg,the limit of quantification was 10μg/kg,the recovery rate of standard addition was 89.3%~98.7%,and the relative standard deviation(RSD)was 3.01%~4.42%.This method was suitable for the qualitative and quantitative detection of 9,10-anthraquinone in tea packaging paper.