基质分散固相萃取-气质联用内标法测定饮料中邻苯二甲酸酯  

Detection of phthalates in beverage by using gas chromatography-mass spectrometry internal standard method with QuEChERS methods

作　　者：郑三燕[1] 陈珞洛[1] 李小东[1] 胡宁恩 林彩琴[1] ZHENG Sanyan;CHEN Luoluo;LI Xiaodong;HU Ningen;LIN Caiqin(Wenzhou Center for Disease Control and Prevention,Zhejiang 325000,China)

机构地区：[1]温州市疾病预防控制中心

出　　处：《海峡预防医学杂志》2019年第5期15-17,74,共4页Strait Journal of Preventive Medicine

基　　金：温州市公益性社会发展(医疗卫生)科技项目(No.Y20160488)

摘　　要：目的建立基质分散固相萃取(SPE,QuEChERS)-气质联用内标法测定饮料中邻苯二甲酸酯方法,并用于饮料中邻苯二甲酸酯类物质(PAEs)测定。方法样品乙腈提取,加氯化钠混匀,离心取上清液,加PSA,无水硫酸镁净化,气质选择离子测定,内标法定量。结果 16种邻苯二甲酸酯类物质在20~1 000μg/L内线性关系良好,相关系数0.999以上。平均回收率86.2%~118.0%,RSD为4.2%~10.2%,检出限0.02~0.05 mg/kg。饮料中检出DEP、DIBP、DBP和DEHP 4种组分,总检出率62.9%(51/81),含量范围8~9 000μg/kg。其中袋装饮料中DBP检出率达64.5%(20/31),浓度最高达9 000μg/kg,DEHP检出率达100.0%(31/31)。结论该方法回收率与精密度均符合要求,操作简单、方便,可用于不同基质饮料中邻苯二甲酸酯的检测。塑料包装特别是街头小摊廉价包装材料对饮料的污染问题不容忽视,要加强监管。Objective To establish a method for detecting phthalates in beverage by using gas chromatography-mass spectrometry(GC-MS) combined with stable isotope internal standard and matrix dispersion solid phase extraction methods(SPE;quick,easy,cheap,effective,rugged,safe,QuEChERS),the PAEs in beverage were detected by the method. Methods The samples were extracted by acetonitrile and added with NaCl. Centrifugal supernatant fluid was purified with MgSO4+PSA adsorbents. The phthalates were qualified by internal standard in the selected ion monitoring(SIM) mode. Results Totally 16 kinds of PAEs showed good linearity in 20-1 000 μg/L,r≥0.999. The recovery rates were 86.2%-118%,and the relative standard deviations(RSD) were 4.2%-10.2%. The limit of detection was 0.02-0.05 mg/kg. DEP,DIBP,DBP and DEHP were detected in beverages. The total detection rate was 62.9%(51/81), and the content range was from 8 to 9000 μg/kg. The detection rate of DBP in bag drinks was 64.5%(20/31), higher concentration was up to 9000 μg/kg and the detection rate of DEHP was 100.0%(1/31). Conclusion The recovery rate and precision of the method meet the requirements. The method is simple and convenient,and can be applicable to detect phthalates for different kinds of beverage. The contamination of beverage by plastic packaging can not be ignored, the supervision and administration should be strengthened, especially for the small street stalls with cheap packaging beverage.

关 键 词：饮料 基质分散固相萃取(SPE QuEChERS) 气质联用仪(GC-MS) 邻苯二甲酸酯物质(PAEs) 

分 类 号：R155.5[医药卫生—营养与食品卫生学]