气相色谱-质谱法测定微胶囊粉剂中18种邻苯二甲酸酯  

Determination of 18 phthalate estersinpowder of microencapsulated oil by gas chromatography-mass spectrometer

作　　者：陆姝欢 柴莎莎 程思 肖敏 周强 杨刚 汪锋 汪志明 李翔宇 

机构地区：[1]嘉必优生物技术(武汉)股份有限公司,武汉430073 [2]湖北省营养化学品生物合成工程技术研究中心,武汉430223 [3]中国科学技术大学,合肥230026 [4]中国科学院合肥物质科学研究院等离子体物理研究所,合肥230031

出　　处：《中国食品添加剂》2017年第12期182-191,共10页China Food Additives

基　　金：国家高技术研究发展计划(863计划)项目资助(No.2014AA021703)

摘　　要：建立了二十二碳六烯酸(DHA)和二十碳四烯酸(ARA)微胶囊粉剂中18种邻苯二甲酸酯类塑化剂的分析方法。考察了不同溶剂和不同净化方式,对前处理的条件进行了优化,最终前处理方法为选用v(乙酸乙酯)∶v(环己烷)=1∶1提取两次,离心后取上清氮吹干,甲醇复溶后冷冻1h,再冷冻离心除杂质。16种邻苯二甲酸酯的方法线性范围为0.5~10 mg/L,邻苯二甲酸二异壬酯(DINP),邻苯二甲酸二异癸酯(DIDP)线性范围为5~100 mg/L,相关系数均大于0.998,加标样品的平均回收率为69.4%~112.6%,RSD(n=6)为1.3%~8.4%。该方法前处理过程简单、溶剂用量小、满足检测需要,可用于不同种类微胶囊粉剂中邻苯二甲酸酯类增塑剂的测定。A gas chromatography mass-spectrometric （GC MS）method for the determination of 18 PAEs in ARA and DHA microencapsulated powder was developed. The solvent of extraction and clean-up methods were investigated and the pretreatment methods were optimized. The clean-up method was ： extracting the powder twice by v （Ethyl acetate） ： v （Cyclohexane） =1 ： 1, the liquid extracts was dried with nitrogen after centrifuge, then redissolved and frozen for 1 hr to removed impuritiesby frozen centrifugation. The calibration curves of 16 PAEs were linear in the range of 0.5 - 10mg/L, and the calibration curves of DINP and DIDP were linear in the range of 5 -100mg/L with correlation coefficients more than 0.998.The average recoveries of the spiked samples were in the range of 67.4% - 112.6% with RSDs （n=6） of 5.3% - 9.4%.The method was simple, accurate and reproducible.It could meet the needs of detection anddetermination of phthalate esters in different kinds of microencapsulated powder.

关 键 词：二十二碳六烯酸 二十碳四烯酸 微胶囊粉剂 塑化剂 气相色谱-质谱 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.7[轻工技术与工程—食品科学与工程]