液相色谱-串联质谱法同时测定食品中10种酚汀类化合物

Simultaneous determination of ten oxyphenisatin derivatives in food by liquid chromatography-tandem mass spectrometry method

建立高效液相色谱-串联质谱法快速测定固体饮料、果冻及果蔬汁饮料三种食品基质中双辛酚丁等10种酚汀类化合物的分析方法。样品使用60%乙腈提取,采用Agilent pursuit C18色谱柱(2.1 mm×100 mm,1.8μm)分离,以10 mmoL/L乙酸铵溶液-乙腈为流动相进行梯度洗脱,通过电喷雾离子源的正负离子扫描模式对三种食品基质中的酚汀类化合物进行定性定量检测。研究结果表明:10种化合物在1.00〜50.0μg/L浓度范围内具有良好的线性关系(r^(2)均大于0.997),检出限均为10.0μg/kg,定量限均为20.0μg/kg,在低、中、高3水平加标,其回收率为80.1%〜106%,相对标准偏差RSD为1.20%〜6.33%(n=6)。该方法专属性好,灵敏度高,前处理简单快速,适用范围广,可用于不同食品基质中非法添加双辛酚丁等10种酚汀类化合物的快速筛查和定量测定。

A liquid chromatography-tandem mass spectrometry(LC-MS/MS)analytical method was established for the rapid determination of ten oxyphenisatin derivatives(including oxyphenisatin diacetate)in three food matrices of solid beverages,jellies,and fruit and vegetable juice beverages.The samples were extracted with 60%acetonitrile and separated by Agilent pursuit C18 column(100 mm×2.1 mm,1.8μm).The separation was based on gradient elution mode,using a mixture of 10 mmol/L ammonium acetate solution and acetonitrile as the mobile phase.Qualitative and quantitative analysis of oxyphenisatin derivatives in the three food matrices was conducted using positive and negative ion scanning modes via electrospray ionization source.The research results showed that the ten compounds exhibited good linearity in the concentration range of 1.00〜50.0μg/L(r^(2)>0.997).The limits of detection(LODs)were 10.0μg/kg and the limits of quantitation(LOQs)were 20.0μg/kg.The recovery rates ranged from 80.1%to 106%when spiked at low,medium,and high levels,with relative standard deviations(RSD)of 1.20%to 6.33%(n=6).This method demonstrated excellent specificity,high sensitivity,simple and rapid sample preparation,wide applicability,it can be utilized for the rapid screening and quantitative determination of 10 phenanthrene compounds including oxyphenisatin diacetate illegally added in different food matrices.