Determination of furan levels in commercial samples of baby food from Brazil and preliminary risk assessment

Commercial baby food samples available on the Brazilian market (n = 31) were analysed for furan content using a gas chromatography-mass spectrometry method preceded by solid-phase microextraction. A limit of detection of 0.7 µg kg^?1, a limit of quantitation of 2.4 µg kg^?1, mean recoveries varying from 80% to 107%, and coefficients of variation ranging from 5.6% to 9.4% for repeatability and from 7.4% to 12.4% for within-laboratory reproducibility were obtained during an in-house validation. The levels of furan found in the samples were from not detected to 95.5 µg kg^?1. Samples containing vegetables and meat showed higher furan levels as compared with those containing only fruits. An exposure assessment showed furan intakes up to 2.4 µg kg^?1 body weight day^?1 (99th percentile) for babies fed exclusively with commercial baby foods. Margins of exposure obtained from intakes estimated in this work indicated a potential public health concern.     

同时蒸馏萃取法和固相微萃取法分析棕榈油与菜籽油复合火锅底料中的风味物质

采用同时蒸馏萃取法和固相微萃取法对棕榈油与菜籽油复合火锅底料中的挥发性风味物质进行提取,并通过气相色谱-质谱联用分析及鉴定。采用2 种方法共鉴定出82 种化合物,其中包括醇类17 种、醛类15 种、酯类9 种、萜烯类16 种、酮类5 种、烃类13 种和其他化合物7 种。其中采用同时蒸馏萃取法检测出58 种化合物,采用固相微萃取法检测出41 种化合物,2 种方法检测出的化合物均以芳樟醇相对含量最大,其次为茴香脑。     

南果梨采后20℃储藏期香气成分变化

采用固相微萃取装置提取香气成分,用气相色谱质谱联用法测定南果梨采后20℃储藏过程中香气成分的变化。结果表明,南果梨采后储藏的前10d,香气成分种类仅为6 种;15d 时,释放香气成分的种类为13 种;20d 时为18 种,达到最多种;25d 时反而减少,仅为12 种。从南果梨中共检测鉴定出19 种化学成分,20d 时主要为：乙酸乙酯(1.49%)、丁酸乙酯(7.48%)、2- 甲基丁酸乙酯(1.43%)、己酸甲酯(1.46%)、己酸乙酯(41.76%)、乙酸己酯(11.78%)、2- 辛烯酸乙酯(1.07%)、辛酸乙酯(6.73%)、和α - 法呢烯(21.6%)。     

采用HS-SPME-GC-MS法对玫瑰饮品香气成分的定量研究

为优化玫瑰饮品酿制工艺,采用顶空固相微萃取-气相色谱质谱联用仪分析了其中19种主要芳香成分,包括芳香族、萜类及其衍生物和烷烃类物质。通过优化各种参数,并结合标准加入法定量,该方法的相关系数为0.990 1～0.999 5,精密度为0.88%～15.21%,检出限为0.02～13.32μg/L,回收率为83.93%～112.02%,表明该法准确可靠。利用该法检测了5种不同种类的玫瑰饮品,发现各成分的含量虽不同,但每种化合物都是在一定范围内变化。β-苯乙醇是最主要的成分(占78.55%～96.03%),含量为64 318.00～195 203.47μg/L;其次是香茅醇、甲基丁香酚、丁子香酚和香叶醇,其各自比例都在0.21%～6.14%,含量为170.01～7 005.90μg/L;再次是乙酸香茅酯、橙花醇、玫瑰醚和橙花叔醇,其含量为数十至300μg/L;其他化合物如部分萜类、烷烃类物质,由于它们的难溶性导致其含量很低,在数十个μg/L甚至1μg/L以下。经统计分析发现,5种玫瑰饮品中化合物含量无显著性差异,但通过聚类分析发现饮料2、3、5总体上最为相似。     

食用油脂中挥发性卤代烃的HS-SPME-GC联用分析

目的：建立进出口油脂中挥发性卤代烃(VHHs)的顶空-固相微萃取-气相色谱(HS-SPME-GC)联用分析方法。方法：采用Supelco公司5种SPME纤维头对食用油脂进行顶空萃取,比较不同萃取纤维的萃取效率,分别考察萃取温度、时间、顶空体积等对萃取效果的影响。用毛细管色谱柱分离萃取成分、气相色谱-电子捕获检测器(GC-ECD)进行检测。结果：优选的SPME纤维头为75μm碳分子筛-聚二甲基硅氧烷(CAR/PDMS)。于15mL顶空萃取瓶中加入9mL食用油,在60℃恒温水浴中萃取30min后,290℃解吸3min进行GC分析。方法检测限为0.02～1.4ng/mL,回收率在89%～105%之间,相对标准偏差(RSD)小于8.5%(n=5)。结论：该方法具有操作简便、快捷、灵敏度高、检测限低、不使用有机溶剂等特点,适合于食用油脂中挥发性卤代烃的检测。     

单滴微萃取-气相色谱法测定塑料食品包装浸出液中邻苯二甲酸酯类物质

建立了基于单滴微萃取(SDME)结合气相色谱法测定塑料食品包装浸出液中3种邻苯二甲酸酯类物质含量的新方法.研究了萃取溶剂、萃取时间及搅拌速度等因素对萃取效率的影响,确定萃取的最佳条件:以1.4 μL二甲苯为萃取剂,萃取时间为20 min,萃取温度为40℃,搅拌速度为200 r/min.在最优条件下,该方法的线性范围为0.1～100 μg/mL,检出限为0.01 μg/mL,实际样品的加标回收率为97％～113.9％.本法具有简单、快速和成本低等特点.     

顶空固相微萃取结合气相色谱-质谱联用法对3种洋葱挥发性风味成分的分析

为研究洋葱挥发性成分,利用顶空固相微萃取法提取洋葱的挥发性风味成分,通过气相色谱-质谱联用法分析测定,以总峰面积和化合物个数为指标考察萃取纤维头、萃取温度、萃取时间和解吸时间4个因素对萃取效果的影响,得出最优萃取条件为:萃取纤维头50/30 μm DVB/CAR/PDMS,萃取温度60 ℃,萃取时间60 min,解吸时间5 min。利用最优萃取条件对三种色泽洋葱挥发性风味成分进行分析鉴定。结果表明:三种色泽洋葱共鉴定得到挥发性风味物质61种,其中白皮、红皮、黄皮洋葱分别测到37、40、49种挥发性成分,相对含量分别占流出组分总量的70.29%、81.92%、79.03%。61种挥发性成分中含硫化合物27种、醛类13种、醇类13种、酮类4种,其他4种。三种色泽洋葱的共有挥发性成分有22种,其中含硫化合物占比较大,特别是二异丙基二硫醚和(E)-1-丙烯基-2-丙烯基二硫醚相对含量的总和在三种色泽洋葱的挥发性成分中占比率都超过了20%,对形成洋葱特征风味贡献较大。红皮和黄皮洋葱的含硫化合物的相对含量远高于白皮洋葱,红皮洋葱中2-甲基-2-戊烯醛相对含量高于白皮和黄皮洋葱。     

Characterisation of volatile compounds in Tunisian fenugreek seeds

In this study, we intend to develop a simple and fast analytical procedure to identify the volatile compounds implicated in the odour of Tunisian fenugreek (Trigonella foenum-graceum L.) seeds. Two procedures, solvent extraction and static headspace solid-phase microextraction (SHS-SPME), have been used under different conditions. The volatile compounds extracted were systematically identified using gas chromatography–mass spectrometry, based on their mass spectrum and Kovats index on two columns of different polarity. A total of 67 compounds were identified, some of them being reported for the first time in fenugreek seeds (e.g. several pyrazines, 2,5-dimethyl-4-hydroxy-3(2H)-furanone or 1-epi-cubenol). Methanol was found to be the preferred solvent for high and medium boiling point volatile compounds, such as sotolone and nitrogen compounds. For SHS-SPME, the fibre coated with divinylbenzene/carboxen/polydimethylsiloxane 2 cm was the most suitable for extracting volatile compounds from ground seeds. The efficiency of this fibre was confirmed by direct gas chromatography–olfactometry, with a global odour similar to that of fenugreek seeds.     

Effect of reduction of lactose in yogurts by addition of β‐galactosidase enzyme on volatile compound profile and quality parameters

A comparative study between reduced‐lactose yogurts made with added β‐galactosidase (E yogurts) and controls (C yogurts) was performed. The evolution of lactose content, pH, acidity and volatile compounds was measured during fermentation and storage at 5 °C. The hydrolysis percentages of lactose ranged from 75% to 78% in E yogurts and from 10% to 13% in C yogurts at the end of manufacture and stayed without changes throughout storage. There were no significant differences in pH and titratable acidity values among yogurts. A total of 22 volatile compounds were identified. The change in lactose level by the action of β‐galactosidase influenced the production of some volatile compounds derived from this sugar. At the end of fermentation, minor differences in volatile composition were recorded among yogurt samples. During storage, acetaldehyde and diketone levels were always higher in hydrolysed yogurts than their respective controls.