同位素稀释气相色谱-质谱/质谱法测定茶叶中蒽醌残留量  

Determination of anthraquinone residues in tea samples by isotope dilutiongas chromatography-tandem mass spectrometry

作　　者：谢文 黄超群 陈丽 申屠炎 洪灯 楼成杰 谢韵第 何建敏 侯建波 邓晓军[3] 于卓然[3] 

机构地区：[1]浙江省检验检疫科学技术研究院,杭州310016 [2]浙江立德产品技术有限公司,杭州310016 [3]上海出入境检验检疫局,上海200135

出　　处：《分析试验室》2017年第2期177-181,共5页Chinese Journal of Analysis Laboratory

基　　金：浙江省科技厅重大科技专项重点农业项目(2015C12001);上海市科委科研项目(15395810100)资助

摘　　要：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。A method for the determination of anthraquinone in tea sample with GC-MS/MS has been introduced.The isotope internal standard（anthraquinone-D8） was added into the sample.Sample was extracted by n-hexane：acetone（1：1,V/V） solution,cleaned-up with Florisil SPE columns,and then diluted with n-hexane：ethyl ether（8：2,V/V） solution.The samples were separated on HP-5MS capillary column（30 m × 0.25 mm（i.d.）,0.25 μm（film thickness）） with temperature programming,and then detected by SRM mode using one precursor/two product ion transitions.The anthraquinone was quantified by the internal standard method.The results showed the method has good linearity in the range of 0 - 200 g/L with correlation coefficients above 0.9990.The recoveries of green tea,black tea,pu ＇er tea and oolong were between 84.2% - 98.1%,and the relative standard deviations（RSDs） were less than 9.7% at the spiked levels of 0.02,0.04 and 0.08 mg/kg.The limit of quantitation was 0.02 mg/kg.The method is simple,rapid,and accurate,and its performance can meet the requirements of the domestic and international legislation.The method could be applied to confirming residues of anthraquinone in tea samples.

关 键 词：茶叶 气相色谱-质谱/质谱 蒽醌 残留 测定 

分 类 号：TS207.5[轻工技术与工程—食品科学]