分子印迹固相萃取-气相色谱/质谱法测定食用油中9种邻苯二甲酸酯  

Determination of 9 phthalate esters in edible oil by molecular imprinting solid phase extraction and gas chromatography/mass spectrometry

作　　者：洪月玲[1] 何娟 HONG Yue-ling;HE Juan(Physical and Chemical Institute,Zhengzhou Center for Disease Control and Prevention,Zhengzhou,Henan 450007,China)

机构地区：[1]郑州市疾病预防控制中心理化检验所,河南郑州450007 [2]河南工业大学化学化工与环境学院,河南郑州450001

出　　处：《中国卫生检验杂志》2019年第20期2467-2470,2474,共5页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立分子印迹固相萃取与气相色谱/质谱法(GC/MS)联用技术同时测定食用油中9种邻苯二甲酸酯(PAEs)的方法。方法准确称取0.5g桶装食用油于10ml的具塞磨口离心管中,分别加入1ml正己烷和5ml乙腈,超声提取20min,收集上清液。加入5ml乙腈重复提取1次,合并2次提取液,45℃氮气吹至近干,加入6ml乙腈,经自制分子印迹固相萃取柱净化,2ml的甲醇洗脱,洗脱液吹至近干后,用正己烷定容至1ml,供GC/MS测定分析。结果经萃取优化后,9种PAEs的线性范围为0.1μg/ml^10μg/ml,线性关系良好,相关系数(r)为0.9990~0.9995,检出限为0.0015μg/ml^0.0030μg/ml,高、中、低3个水平的加标浓度的回收率为82.5%~102.1%,6次样品测定结果计算相对标准偏差在0.26%~3.41%。结论该聚合物具有化学和热稳定性、可重复实用性和特异性识别能力,该方法是一种准确的、有选择性的、灵敏的痕量组分的样品前处理技术,可以应用于食用油中9种邻苯二甲酸酯类的同时检测。Objective To establish a method for the simultaneous determination of phthalate esters(PAEs)in edible oil used by molecular imprinting solid phase extraction(MISPE)with gas chromatography/mass spectrometry(GC/MS).Methods Firstly,edible oil(0.5 g)was added into 10 ml centrifugal tube,followed by the introduction of 1 ml n-hexane and 5 ml acetonitrile into the tube.The mixture was extracted ultrasonically for 20 min and the extraction procedure was repeated twice.After that,the supernatant was concentrated to nearly dry under nitrogen flow at 45℃,before the residue was reconstituted with 6 ml acetonitrile.The solution was loaded on MISPE column.The PAEs absorbed on the adsorbent were eluted with 2ml of methanol and the eluent was subsequently bubbled with nitrogen to nearly dry.Afterwards,1 ml n-hexane was added to dissolve the residue and vortexed for GC/MS analysis.Results Under the optimum extraction conditions,good linearity was obtained within 0.1μg/ml-10μg/ml and the correlation coefficient(r)was within 0.999 0-0.999 5 for nine PAEs.The limits of detection(LOD)and the limits of quantification(LOQ)were within 0.001 5μg/ml-0.003 0μg/ml and 0.005μg/ml-0.016μg/ml.Satisfied recoveries were within 82.5%-102.1%in low,middle and high level standard addition experiments.The relative standard deviation values(RSDs)were within 0.26%-3.41%in 6 times of sample test.Conclusion The adsorbent exhibits chemical and thermal stability,reusability,and high specific recognition ability.The pretreatment method is accurate,selective,and sensitive to detect trace amount of chemicals,which is suitable for the simultaneous determination of phthalate esters in edible oil.

关 键 词：分子印迹固相萃取 气相色谱/质谱法 邻苯二甲酸酯类 食用油 

分 类 号：R155.5[医药卫生—营养与食品卫生学]