摘要
建立了Qu ECh ERS结合气相色谱-质谱法(GC-MS)快速检测玉米中14种邻苯二甲酸酯类塑化剂(PAEs)的方法。样品经乙腈溶液提取,无水硫酸镁和氯化钠盐析后,经N-丙基乙二胺(PSA)填料、十八烷基键合硅胶(C18)及石墨炭黑(GCB)净化,采用选择离子模式,外标法定量。结果表明:14种PAEs在1~500μg/L范围内,采用基质匹配法绘制标准曲线,线性良好,相关系数在0.9945~0.9995之间;在15、150、500μg/kg的加标水平下,平均回收率为80.0%~109.8%,相对标准偏差均小于9.0%;检出限(S/N=3)与定量限(S/N=10)分别为0.1~2.5和0.13~5.0μg/kg。将该方法应用于6个不同产地的玉米原料检测,结果显示:样品中检出邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二异丁酯、邻苯二甲酸二丁酯和邻苯二甲酸二(2-乙基)己酯此5种塑化剂,且塑化剂含量均低于国标限量标准。该方法高效、快速、灵敏度高,适合于玉米样品的日常监测。
A modified QuEChERS method was developed for the simultaneous determinationn of 14 phthalate esters(PAEs)in corn prior to gas chromatography-mass spectrometry(GC-MS)analysis.All of the PAEs in corn samples were extracted into acetonitrile and salted out by anhydrous Mg SO_4and Na Cl.Then,the PAEs in the supernatant after clean-up by primary secondary amine(PSA),octadecyl silica(C_(18)),and graphitized carbon black(GCB)were subjected to GC-MS analysis.External standard quantification was used to determine the extraction efficiency of each sample.As a result,14 PAEs possessed an excellent linear relation by using matrix-matched curve under 1~500μg/L,and the correlation coefficients were 0.9945~0.9995.The recoveries of 14 PAEs in corn matrixes at three spiked levels of 15,150 and 500μg/kg ranged from 80.0%to109.8%with relative standard deviations below 9.0%.The LODs and LOQs for PAEs,based on S/N of 3 and 10,ranged from0.1 to 2.5μg/kg and 0.13 to 5.0μg/kg,respectively.The applicability of the method was properly validated using six corns,and the results revealed that the dimethyl phthalate(DMP),diethyl phthalate(DEP),diisobutyl phthalate(DIBP),dibutyl phthalate(DBP),and bis(2-methoxyethyl)phthalate(DEHP)were detected in all the samples.The content of PAEs is lower than the standard of GB.Overall,the developed QuEChERS-GC/MS method could be considered as a promising method for routine monitoring of PAEs residue in corn since the procedure was easy,fast,and effective.
作者
孙啸涛
刘淼
曾凤鸣
敖灵
孙宝国
孙金沅
郑福平
黄明泉
李贺贺
SUN Xiao-tao;LIU Miao;ZENG Feng-ming;AO Ling;SUN Bao-guo;SUN Jin- yuan;ZHENG Fu- ping;HUANG Ming- quan;LI He- he(College of Food Engineering and Biotechnology, Tianjin University of Science and Technology, Tianjin 300457, China;Beijing Laboratory for Food Quality and Safety, Beijing Technology and Business University ,Beijing 100048, China;Luzhou Laojiao Co.Ltd. ,Luzhou 646000 ,China)
出处
《食品工业科技》
CAS
CSCD
北大核心
2018年第8期199-204,209,共7页
Science and Technology of Food Industry
基金
国家自然科学基金青年科学基金项目(31601556)
“十三五”国家重点研发计划重点专项(2016YFD0400501)
四川省科技计划项目(2017JZ0012)