MSPE-GC-BID同时测定白酒中16种邻苯二甲酸酯含量  

Simultaneous Determination of 16 Phthalates in Baijiu by MSPE-GC-BID

作　　者：贾鹏禹[1,2] 陈爽 孙蕊 李良玉[1,2] 闫岩[2] 张丽媛 JIA Pengyu;CHEN Shuang;SUN Rui;LI Liangyu;YAN Yan;ZHANG Liyuan(College of Food Science,Heilongjiang Bayi Agricultural University,Daqing 163319,China;National Coarse Cereals Engineering Research Center,Heilongjiang Bayi Agricultural University,Daqing 163319,China;College of Animal Science&Veterinary Medicine,Heilongjiang Bayi Agricultural University,Daqing 163319,China)

机构地区：[1]黑龙江八一农垦大学食品学院,黑龙江大庆163319 [2]黑龙江八一农垦大学国家杂粮工程技术研究中心,黑龙江大庆163319 [3]黑龙江八一农垦大学动物科技学院,黑龙江大庆163319

出　　处：《食品科技》2024年第7期300-307,共8页Food Science and Technology

基　　金：黑龙江八一农垦大学“三纵”科研支持计划项目(ZRCPY202227);黑龙江八一农垦大学学成引进人才科研启动计划项目(XDB202116)。

摘　　要：文章建立了磁固相萃取结合气相色谱-介质阻挡放电等离子体检测器(Barrier discharge ionization detector, BID)对白酒中16种邻苯二甲酸酯含量的检测方法,优化了磁固相萃取条件。该方法采用50.0 mg磁性吸附剂,在50℃下萃取10 min,目标物萃取后经2.0 mL丙酮/乙酸乙酯混合溶液(9:1,V/V),在50℃下解吸15 min后上机检测。气相色谱进样口温度为270℃,色谱分离柱采用CD-5(30 m×0.25 mm×0.25μm,5%苯基-聚二甲基硅氧烷)石英毛细管柱,在程序升温模式下分离组分,BID检测器温度为290℃,放电气体流量为25.0 mL/min,不分流进样体积为1μL。结果表明,16种邻苯二甲酸酯在20.0~3000.0 ng/mL的浓度范围内线性关系良好,相关系数为0.9989~0.9998,加标回收率为62.4%~127.1%,检出限为0.12~0.49 ng/mL。所建方法操作简单、准确度高、精密度好,可用于白酒样品中16种邻苯二甲酸酯的测定。A method of magnetic solid phase extraction combined with gas chromatography-barrier discharge ionization detector(MSPE-GC-BID)was established for the determination of 16 phthalates in Baijiu,and the conditions of magnetic solid phase extraction were optimized.The method used 50.0mg magnetic adsorbent and extracted at 50℃for 10 min.Then the target substances were desorbed at 50℃for 15 min in a 2.0 mL mixture of acetone/ethyl acetate solution(9:1,V/V)and detected on the system.The inlet temperature of gas chromatography was 270℃,and the chromatographic separation column used a CD-5(30 m×0.25 mm×0.25μm,5%phenyl-polydimethylsiloxane)quartz capillary column.The components were separated under programmed temperature mode,and the BID detector temperature was 290℃.The discharge gas flow rate was 25.0 mL/min,and the volume of non split injection was 1μL.The results showed that there was a good linear relationship among the 16 phthalates in the concentration range of 20.0 ng/mL to 3000.0 ng/mL,with correlation coefficients between 0.9989 and 0.9998,recovery rates of 62.4%to 127.1%,and detection limits of 0.12 ng/mL to 0.49ng/mL.The method was simple,accurate and precise,and could be used for the determination of 16phthalates in Baijiu samples.

关 键 词：磁固相萃取 气相色谱 介质阻挡放电等离子体检测器 邻苯二甲酸酯 白酒 

分 类 号：TS207.5[轻工技术与工程—食品科学]