磁性固相萃取-气相色谱-串联质谱法测定市售酒中16种邻苯二甲酸酯  

Determination of 16 types of phthalic acid esters in commercial liquors by magnetic nanoparticles solid-phase extraction combined with gas chromatography-tandem mass spectrometry

作　　者：王芳[1] 杨凤华[1] 邵国健[2] 胡明友[2] 王晔 WANG Fang;YANG Fenghua;SHAO Guojian;HU Mingyou;WANG Ye(Department of Education and Quality Management,Huzhou Center for Disease Control and Prevention,Zhejiang,Huzhou 313000,China;Huzhou Center for Disease Control and Prevention,Zhejiang,Huzhou 313000,China)

机构地区：[1]湖州市疾病预防控制中心科教质管科,浙江湖州313000 [2]湖州市疾病预防控制中心,浙江湖州313000

出　　处：《预防医学》2022年第8期855-860,共6页CHINA PREVENTIVE MEDICINE JOURNAL

基　　金：湖州市科学技术局公益性应用研究项目(2020GYB09)。

摘　　要：目的建立基于吡咯修饰磁性纳米材料的磁性固相萃取-气相色谱-串联质谱法(GC-MS/MS),测定市售酒中16种邻苯二甲酸酯(PAEs)。方法通过水热合成Fe3O4磁核,采用化学氧化法制备聚吡咯修饰磁性纳米材料,以酒精度10%,萃取时间20 min,乙酸乙酯洗脱10 min对啤酒、葡萄酒、黄酒和白酒样品进行磁性固相萃取,加入1g氯化钠减少乳化效应。采用DB-5MS毛细管色谱柱(30 m×250μm,0.25μm)分离,在电子轰击电离(EI)和动态多反应监测(dMRM)模式下,采用GC-MS/MS检测16种PAEs,外标法定量。测定16种PAEs的标准曲线、检出限、加标回收率和精密度,对方法进行评价。结果吡咯以聚合物的形式成功接枝在磁性纳米颗粒的表面,PPy@Fe3O4表征良好。基质效应和乳化效应不明显。16种PAEs在50~5000 ng/mL内线性关系良好,r值为0.9995~0.9999。在100、500和1000μg/kg水平下,16种PAEs的加标回收率为71.61%~110.50%,相对标准偏差为3.78%~7.41%,检出限为0.02~1.47μg/kg。共检测市售酒样品40份,检出PAEs 20份;啤酒、葡萄酒、黄酒和白酒的检出率分别为30.00%、60.00%、40.00%、70.00%。结论本方法灵敏度高,基质效应和乳化效应不明显,聚吡咯修饰磁性复合纳米粒子对酒类样品中PAEs具有良好的吸附性,可应用于多种酒类样品的PAEs检测。Objective To develop a magnetic solid-phase extraction combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)based on pyrrole-modified magnetic nanoparticles to determine 16 types of phthalic acid es⁃ters(PAEs)in commercial liquors.Methods Fe3O4 magnetic nuclei were prepared by hydrothermal synthesis,and the polypyrrole-modified magnetic nanomaterials were prepared with the chemical oxidation method.Magnetic solid-phase ex⁃traction of beer,grape wine,rice wine and Chinese spirits was performed at 10%alcohol by volume,extraction duration of 20 min and ethyl acetate elution of 10 min,followed by addition of 1 g NaCl for reduction of emulsification effect.The 16 types of PAEs were determined using GC-MS/MS with DB-5MS capillary column(30 m×250μm,0.25μm)un⁃der the mode of electron impact ionization(EI)and dynamic multiple reaction monitoring(dMRM),with quantitative anal⁃ysis using the external standard method.The standard curve,detection limit,spike recovery rate and precision of GC MS/MS for determination of 16 types of PAEs were evaluated.Results Pyrrole was successfully embedded onto the sur⁃face of magnetic nanoparticles in the form of polymer,and the magnetic nanoparticles modified by polypyrrole were well characterized,showing unapparent matrix and emulsification effects.There was a good linear relationship for the 16 types of PAEs at 50 to 5000 ng/mL(r=0.9995-0.9999),and the spike recovery rate of 16 types of PAEs ranged from 71.61%to 110.50%at 100,500 and 1000μg/kg,with relative standard deviations of 3.78%to 7.41%,detection limits of 0.02 to 1.47μg/kg.PAEs were detected in 20 out of 50 liquor samples,with 30.00%,60.00%,40.00%and 70.00%detection rates in beer,grape wine,rice wine and Chinese spirits,respectively.Conclusions This method is sensitive to determine 16 types of PAEs in liquor samples,with unapparent matrix and emulsification effects,and the polypyrrole-modified magnetic composite nanoparticles present high adsorption of PAEs in liquor samples,which is feasi⁃ble for mo

关 键 词：磁性纳米材料 酒 邻苯二甲酸酯 气相色谱-串联质谱 

分 类 号：R994.4[医药卫生—毒理学]