色谱

色谱 ›› 2013, Vol. 31 ›› Issue (12): 1232-1239.DOI: 10.3724/SP.J.1123.2013.07019

• 技术与应用 • 上一篇    

固相微萃取-气相色谱/质谱法测定果汁及茶饮料中的10种光引发剂

刘芃岩, 陈艳杰, 赵春霞, 田磊   

  1. 河北大学化学与环境科学学院, 河北 保定 071002
  • 收稿日期:2013-07-15 修回日期:2013-08-30 出版日期:2013-12-28 发布日期:2013-12-05
  • 通讯作者: 刘芃岩
  • 基金资助:

    河北省科技支撑计划项目（12220402D）；保定市科技支撑计划项目（08J03）

Determination of ten photoinitiators in fruit juices and tea beverages by solid-phase micro-extraction coupled with gas chromatography/mass spectrometry

LIU Pengyan, CHEN Yanjie, ZHAO Chunxia, TIAN Lei   

  1. College of Chemistry & Environmental Science, Hebei University, Baoding 071002, China
  • Received:2013-07-15 Revised:2013-08-30 Online:2013-12-28 Published:2013-12-05

PDF

296

被引次数

15

摘要：

建立了用固相微萃取结合气相色谱/质谱（GC/MS）检测13种果汁饮料和3种茶饮料中10种光引发剂的方法。通过正交试验筛选对萃取过程影响较大的因素，再通过单因素试验进一步优化，确定最佳的操作条件。样品经萃取后，在GC/MS进样口解吸3 min，经HP-5MS色谱柱分离，以选择离子方式监测，外标法定量。为消除基质的干扰，以样品基质加标做工作曲线，线性范围为0.3~60 μg/L，检出限为3~16 ng/L。分别对4个不同加标水平的样品平行测定5次，相对标准偏差均小于14.5%。对不同品牌、不同种类的16种盒装饮料进行了测定，所有样品中全部检出二苯甲酮，部分样品中检出对二甲氨基苯甲酸异辛酯、2-异丙基硫杂蒽酮、4-甲基二苯甲酮、1-羟基环己基苯基甲酮、2-氯噻吨酮。该方法操作简单、灵敏度高、无污染，可对10种光引发剂同时测定。该研究结果为从包装材料迁移至饮料中的光引发剂的测定提供了参考。

关键词: 固相微萃取, 光引发剂, 果汁, 气相色谱/质谱, 饮料

Abstract:

A method for the determination of ten photoinitiators (PIs), benzophenone, ethyl 4-dimethylaminobenzoate, 1-hydroxycyclohexyl-phenylketone, 4-methylbenzophenone, 2-ethylhexyl-4-dimethylaminobenzoate, 4-chlorobenzophenone, 2-chlorothioxanthone, 2-isopropylthioxanthone, 2,2-dimethoxy-2-phenylacetophenone, methyl 2-benzoylbenzoate, in 13 kinds of fruit juice and 3 kinds of tea beverage has been established, using solid-phase micro-extraction (SPME) combined with chromatography/mass spectrometry (GC/MS). At first, the major factors of SPME, extraction time and temperature, were studied through orthogonal experiment. Then the optimal operation conditions were obtained via the refinement of various factors. After the sample was extracted by SPME, it was desorbed for target analytes in sampling inlet for 3 min, and separated on an HP-5MS column, then detected by MS in selected ion monitoring mode, and quantified through calibration curve. The working curves were obtained using sample matrix in order to eliminate the matrix interference. The linear range was from 0.3 μg/L to 60 μg/L and the detection limit range was from 3 ng/L to 16 ng/L. The samples were determined five times with four different spiked levels individually and the relative standard deviations of all the samples were less than 14.5%. This determination method was applied in 16 kinds of packed beverages with different brands and different species. Benzophenone had been detected from all the samples. 4-Methylbenzophenone, 2-ethylhexyl-4-dimethylaminobenzoate, 2-isopropylthioxanthone, 1-hydroxycyclohexyl-phenylketone and 2-chlorothioxanthone had been detected from a portion of samples. Simultaneous determination was achieved for the ten PIs. These results provide a reference to determine the PIs migrated from packing materials in beverage. This method is simple, high sensitive and non-polluting.

Key words: beverages, fruit juices, gas chromatography/mass spectrometry (GC/MS), photoinitiators, solid-phase micro-extraction

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