首页|MSPE-GC-BID同时测定白酒中16种邻苯二甲酸酯含量

MSPE-GC-BID同时测定白酒中16种邻苯二甲酸酯含量

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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×0.25 μm,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1 μL.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.
Simultaneous Determination of 16 Phthalates in Baijiu by MSPE-GC-BID
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 50.0 mg 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×0.25 µm,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 1 μL.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 0.49 ng/mL.The method was simple,accurate and precise,and could be used for the determination of 16 phthalates in Baijiu samples.

magnetic solid phase extractiongas chromatographybarrier discharge ionization detectorphthalatesBaijiu

贾鹏禹、陈爽、孙蕊、李良玉、闫岩、张丽媛

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黑龙江八一农垦大学食品学院,黑龙江大庆 163319

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

黑龙江八一农垦大学动物科技学院,黑龙江大庆 163319

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

黑龙江八一农垦大学"三纵"科研支持计划项目黑龙江八一农垦大学学成引进人才科研启动计划项目

ZRCPY202227XDB202116

2024

食品科技
北京市粮食科学研究所

食品科技

CSTPCD北大核心
影响因子:0.622
ISSN:1005-9989
年,卷(期):2024.49(7)