QuEChERS-GC-MS联用法检测大麦中14种邻苯二甲酸酯类塑化剂及基质效应的影响

发布时间：2018-03-13 01:18

本文选题：大麦　切入点：QuEChERS　出处：《食品科学》2016年24期 　论文类型：期刊论文

【摘要】：采用QuEChERS结合气相色谱-质谱联用技术建立检测大麦中14种邻苯二甲酸酯类(phthalate esters,PAEs)塑化剂的高效、准确方法。样品粉碎、过80目筛,溶于p H 2的水溶液。采用乙腈提取,无水硫酸镁和氯化钠盐析,经十八烷基键合硅胶(C_(18))净化,C_(18)/大麦比例为50 mg/g;以提取后添加法对大麦中PAEs检测的基质效应评估。结果表明,大麦基质对PAEs均存在基质增强效应,增强比为41.0%~78.1%,采用基质匹配-标准曲线法能较好消除基质效应的影响,提高定量准确度;14种PAEs在大麦基质3个加标水平(15、150μg/kg和500μg/kg)的平均回收率为73.8%~120.1%,相对标准偏差均小于10%;检出限(3倍)与定量限(10倍)分别为0.1~2.5μg/kg和0.13~5.0μg/kg。应用该方法对6个不同产地的大麦原料检测,结果显示: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(dibutyl phthalate,DBP)和邻苯二甲酸二(2-乙基)己酯(bis(2-ethylhexyl)phthalate,DEHP)在6个样品中均有检出,含量存在差异;参照GB 9685—2008《食品容器、包装材料用添加剂使用卫生标准》规定,本次检出的大麦样品中DBP、DEHP含量均低于允许最大残留限量标准。
[Abstract]:QuEChERS and gas chromatography-mass spectrometry (GC-MS) were used to establish an efficient and accurate method for the determination of 14 phthalate ester phthalate phthalate (PAEs) plasticizers in barley. The samples were pulverized, sifted over 80 mesh and dissolved in pH 2 aqueous solution. Acetonitrile was used to extract the plasticizer. Anhydrous magnesium sulfate and sodium chloride were salted out and purified by 18 alkyl bonded silica gel. The ratio of C / barley was 50 mg / g. The matrix effect of PAEs detection in barley was evaluated by adding extraction method. The results showed that the matrix enhancement effect of barley substrates on PAEs was observed. The enhancement ratio is 41.0 / 78.1.The matrix matching standard curve method can better eliminate the effect of matrix effect. The average recoveries of 14 kinds of PAEs in barley substrates were 73.8% and 120.1, respectively. The relative standard deviations were less than 10%; the detection limit was 3 times and the quantitative limit was 0.1 渭 g / kg and 0.135.0 渭 g / kg, respectively. Examination of barley raw materials from the same origin, The results showed that dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, dibutyl phthalate (DBP) and diethylhexylphthalate (DEHP) were detected in 6 samples. With reference to the hygienic standard for the use of additives in packaging materials, the DBP DEHP contents in barley samples were all lower than the allowable maximum residue limit standard.
【作者单位】：北京工商大学食品学院北京食品营养与人类健康高精尖创新中心北京市食品风味化学重点实验室北京食品质量与安全实验室;
【基金】：国家自然科学基金青年科学基金项目(31601556;31301466) 北京市教委科技计划重点项目(KZ201410011015) 2016年研究生科研能力提升计划项目
【分类号】：S512.3;O657.63

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