气液微萃取技术联用气相色谱-质谱法快速检测包装食品中15种邻苯二甲酸酯
目的 建立气液微萃取技术(gas liquid microextraction, GLME)联用气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)快速检测包装食品中15种邻苯二甲酸酯(phthalic acid esters, PAEs)的方法。方法 称取0.1 g样品放入GLME中进行萃取、净化、浓缩, 加入20 ng仪器内标, 定容至100 μL, 利用GC-MS对5种包装食品中15种PAEs的浓度进行检测。结果 样品中检测出邻苯二甲酸二异丁酯(diisobutyl phthalate, DIBP)、邻苯二甲酸二丁酯(dibutyl phthalate, DBP)、邻苯二甲酸二甲氧基乙酯(dimethoxyethyl phthalate, DMEP)、邻苯二甲酸二(2-丁氧基)乙酯(bis(2-butoxyethyl) phthalate, DBEP)、邻苯二甲酸二环己酯(dicyclohexyl phthalate, DCHP)、邻苯二甲酸二(2-乙基)己酯(dioctyl phthalate, DEHP)等6种塑化剂, 其中DIBP、DBP、DMEP、DCHP、DEHP等5种塑化剂的检测率达到100%。该方法可以在5 min内完成萃取、净化、浓缩等步骤, 回收率为55.2%~121.9%和相对标准偏差(relative standard deviation, RSD)小于20.0%。结论 本方法实现了对于包装食品中塑化剂的快速检测, 为以后的现场检测塑化剂打下了坚实的基础。
Objective To establish a method for rapid determination of 15 kinds of phthalic acid esters (PAEs) in packaged foods by gas liquid microextraction (GLME) coupled with gas chromatography-mass spectrometry (GC-MS). Methods The sample amount of 0.1 g was directly added to the GLME for extraction, purification and concentration. After adding 20 ng internal standard, the final volume was adjusted to 100 μL and directly injected into GC-MS for analysis of PAEs from 5 kinds of packaged food. Results There were 6 kinds of plasticizers which were detected in the real samples, including diisobutyl phthalate (DIBP), dibutyl phthalate (DBP), dimethoxyethyl phthalate (DMEP), bis(2-butoxyethyl) phthalate (DBEP), dicyclohexyl phthalate (DCHP), dioctyl phthalate (DEHP). The detection rate of DIBP, DBP, DMEP, DCHP and DEHP reached 100%. This method could completed the extraction, purification and concentration steps in 5 minutes, the result showed good recoveries with 55.2%~121.9%, and the relative standard deviations (RSD) were less than 20.0%. Conclusion This method has realized the rapid detection of plasticizer in packaged food, which lays a solid foundation for the field detection of plasticizer.
标题：气液微萃取技术联用气相色谱-质谱法快速检测包装食品中15种邻苯二甲酸酯
英文标题：Rapid detection of 15 kinds of plasticizers in packaged food by gas liquid microextraction coupled with gas chromatography-mass spectrometry
作者：
李婉莹 延边大学理学院,长白山生物资源与功能分子教育部重点实验室
赵锦花 延边大学理学院,长白山生物资源与功能分子教育部重点实验室
蒋世翠 延边大学理学院,长白山生物资源与功能分子教育部重点实验室
石金娥 吉林省食品检验所
李宁 吉林省食品检验所
柴竹林 吉林省食品检验所
李刚 吉林省食品检验所
华蕾 吉林省食品检验所
李东浩 延边大学理学院,长白山生物资源与功能分子教育部重点实验室
中文关键词:包装食品,邻苯二甲酸酯,快速检测,气液微萃取技术,气相色谱-质谱法,
英文关键词:packaged food,phthalic acid esters,rapid detection,gas liquid microextraction,gas chromatography- mass spectrometry,
发表日期：2017-09-06
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