Analytical and Bioanalytical Chemistry ( IF 3.8 ) Pub Date : 2018-03-17 , DOI: 10.1007/s00216-018-0986-x Ivan Notardonato , Elisabetta Salimei , Mario Vincenzo Russo , Pasquale Avino
Baby foods are either a soft, liquid paste or an easily chewed food since babies lack developed muscles and teeth to chew effectively. Babies typically move to consuming baby food once nursing or formula is not sufficient for the child’s appetite. Some commercial baby foods have been criticized for their contents. This article focuses on the simultaneous determination of organophosphorus pesticides and phthalates by means of a method based on ultrasound–vortex-assisted liquid–liquid microextraction coupled with gas chromatography–ion trap mass spectrometry (GC–IT/MS). The protocol developed allowed the determination of six phthalates [dimethyl phthalate, diethyl phthalate, dibutyl phthalate, isobutyl cyclohexyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate] and 19 organophosphorus pesticides. Freeze-dried product samples (0.1-0.2 g) were dissolved in 10 mL of warm distilled water along with 5 μL of an internal standard (anthracene at 10 mg mL-1 in acetone): the choice of extraction solvent was studied, with the most suitable being n-heptane, which is used for phthalate determination in similar matrices. The solution, held for 5 min in a vortex mixer and for 6 min in a 100-W ultrasonic bath to favor solvent dispersion and consequently analyte extraction, was centrifuged at 4000 rpm for 30 min. Then 1 μL was injected into the GC–IT/MS system (SE-54 capillary column; length 30 m, inner diameter 250 μm, film thickness 0.25 μm). All analytical parameters investigated are discussed in depth. The method was applied to real commercial freeze-dried samples: significant contaminant concentrations were not found.
中文翻译:
超声-涡旋辅助液-液微萃取和GC-IT / MS同时测定婴儿食品中的有机磷农药和邻苯二甲酸盐
婴儿食品要么是柔软的液态糊状物,要么是容易咀嚼的食物,因为婴儿缺乏发达的肌肉和牙齿,无法有效地咀嚼。一旦哺乳或配方奶不足以满足孩子的食欲,婴儿通常会开始食用婴儿食品。一些商业婴儿食品因其含量而受到批评。本文着重介绍基于超声-涡流辅助液-液微萃取-气相色谱-离子阱质谱(GC-IT / MS)的方法同时测定有机磷农药和邻苯二甲酸酯的方法。制定的规程允许测定六种邻苯二甲酸酯[邻苯二甲酸二甲酯,邻苯二甲酸二乙酯,邻苯二甲酸二丁酯,邻苯二甲酸环己基异丁酯,邻苯二甲酸苄基丁酯,邻苯二甲酸双(2-乙基己基)]和19种有机磷农药。冷冻干燥的产品样品(0.1-0。-1(在丙酮中为-1):研究了萃取溶剂的选择,最合适的是正庚烷,该庚烷用于在类似基质中测定邻苯二甲酸盐。将溶液在涡旋混合器中保持5分钟,并在100 W超声波浴中保持6分钟,以利于溶剂分散并随后进行分析物提取,将溶液以4000 rpm离心30分钟。然后将1μL注入GC–IT / MS系统(SE-54毛细管柱;长度30 m,内径250μm,膜厚0.25μm)。深入讨论了所有分析参数。该方法已应用于实际的商业冻干样品:未发现明显的污染物浓度。