三重四级杆气质联用法测定水产品中12种碳九芳烃  

Determination of 12 kinds of C9 aromatics in aquatic products by gas chromatography-triple quadrupole mass spectrometry

作　　者：钟建永 张冰泉 谢亚兴 林诗凯 刘少辉 戴明男 李志辉 ZHONG Jianyong;ZHANG Bingquan;XIE Yaxing;LIN Shikai;LIU Shaohui;DAI Mingnan;LI Zhihui(Zhongfang Textile and Apparel Testing(Fujian)Co.Ltd.,Quanzhou 362000,China)

机构地区：[1]中纺检测(福建)有限公司,福建泉州362000

出　　处：《食品与发酵工业》2021年第21期246-252,共7页Food and Fermentation Industries

基　　金：2020年泉州市丰泽区科技计划项目(2020FZ13)。

摘　　要：该文建立了水产品中12种碳九芳烃的三重四级杆气质联用分析测定方法。建立了12种碳九芳烃的多反应监测(multiple reaction monitoring,MRM)方法,得到了12种碳九芳烃的保留时间和MRM质谱参数,并绘制了其总离子流图(total ion chromatography,TIC)。对乙酸乙酯、正己烷、丙酮和正己烷∶丙酮(体积比7∶3)混合溶液共4种有机溶剂提取水产品中目标物的能力进行试验,最后确定以乙酸乙酯为提取溶剂。比较了超声和均质2种提取方式,确定以均质为该方法的提取方式,提取时间2 min。研究了不同净化吸附剂用量对12种碳九芳烃回收率的影响,确定加入的净化吸附剂用量为:0.1 g乙二胺-N-丙基硅烷(primary secondary amine,PSA)、1 g无水硫酸镁、1 g中性氧化铝。结果表明,12种碳九芳烃在质量浓度为0.01~1.0μg/mL线性良好,仪器检出限为0.124~2.502μg/L,定量限为0.413~8.340μg/L,方法检出限为0.248~5.004μg/kg,平均回收率为75%~112%,相对标准偏差(relative standard deviation,RSD)<6.7%,并用建立的方法测定了市场上不同水产品中12种碳九芳烃的含量,结果可靠。该方法可对水产品中的碳九芳烃进行定性定量分析,为地标乃至国标的建立提供参考。The method for the determination of 12 kinds of C9 aromatics in aquatic products by gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)was established.The multiple reaction monitoring(MRM)method of 12 kinds of C9 aromatics was established,and the retention time and MRM mass spectrometric parameters of 12 kinds of C9 aromatics were obtained.The total ion chromatography(TIC)of 12 kinds of C9 aromatics was also plotted.The four organic solvents,ethyl acetate,n-hexane,acetone and n-hexane:acetone(7:3)mixed solution,were tested for their ability to extract the targets in aquatic products.Ethyl acetate was used as the final extraction solvent.Two extraction methods of ultrasonic and homogenization were compared,and the homogenization-based extraction method was determined.The extraction time was 2 min.The dosage of purification adsorbent was 0.1 g primary secondary amine(PSA),1 g anhydrous magnesium sulfate,1 g neutral alumina.The results showed that 12 kinds of C9 aromatics were detected in a linear dynamic range of 0.01-1.0μg/mL.The limits of instrument detection(LOID),limits of quantitation(LOQ)and limits of method detection(LOMD)were 0.124-2.502μg/L,0.413-8.340μg/L and 0.248-5.004μg/kg respectively.The average recoveries were in the range of 75%-112%and the relative standard deviations(RSD)were below 6.7%.The method was used to determine the content of 12 kinds of C9 aromatics in different aquatic products.It provided reference for the establishment of landmarks and even national standards.

关 键 词：碳九芳烃 三重四级杆气质联用 水产品 多反应监测 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]