Determination of furan in jarred baby food purchased from the Spanish market by headspace gas chromatography-mass spectrometry (HS-GC-MS)

The aim of this paper is to offer a method based on headspace gas chromatography-mass (HS-GC-MS) spectrometry technique in-house validated and use to estimate furan concentrations in jarred baby-food samples purchased from the Spanish market. The validation was performed according to ISO 17025 and European Food Safety Authority (EFSA) requirements and the results obtained (limit of detection (LOD) = 0.05 µg kg^?1; limit of quantification (LOQ) = 4 µg kg^?1, lowest validated level; relative standard deviation (RSD) = 3.1–10.5%; recoveries = 85.4–101.5%) confirm that this method is fit for the routine analysis of furan in jarred baby food control. Furan was analysed in 39 different baby-food samples and the mean levels varied between 64.6 µg kg^?1 (rice and chicken samples) and less than or equal to the LOQ (fruit-based samples). The mean concentrations found for the different matrices were 5.0, 37.8, 25.2, 33.8 and 30.5 µg kg^?1 for fruit, vegetables, meat/vegetables, fish/vegetables and dairy-containing baby foods, respectively. According to the statistical analyses, fruit-based baby-food samples had significantly lower concentrations of furan. Mean values for the other matrices were at least five times higher, and this is in accordance with the levels reported in other studies.     

Furan in commercial baby foods from the Spanish market: estimation of daily intake and risk assessment

ABSTRACT

The occurrence of furan in commercial baby food samples from the Spanish market was evaluated using an automated headspace solid-phase microextraction method coupled to gas chromatography-mass spectrometry (HS-SPME-GC-MS). A total of 76 baby food samples including infant formula, baby cereals, fruit in cans and/or jars, vegetables, meat, and fish, were surveyed for furan content. The lowest concentration of this compound was found in infant formula (<0.02–0.33 ng ml^?1), and cereal-based food (0.15–2.1 ng g^?1) while baby food containing fish showed the highest concentrations (19–84 ng g^?1). Following recommendation of the European Food Safety Authority (EFSA), the effect on furan content was evaluated of consumer home preparation of foods, heating and handling. Furan concentrations were reduced by up to 35% when samples were heated in a dish using microwave oven and by up to 53% when a hot water bath was used. Finally, we estimated the furan intake from baby food consumption (0.002–1.18 µg kg^?1 body weight day^?1) and we calculated the margin of exposure (MOE) from samples as purchased and also after home preparation of the food. For infant formula and cereal baby foods, the MOEs (26,278–412,776) indicated no infant health concern or priority, while for meat and fish-based baby foods the values pointed to a potential public health risk, even considering the furan losses during preparation at home.     

Effect of cooking or handling conditions on the furan levels of processed foods

The aim of this study was to investigate the possible effects of cooking or handling conditions on the concentration of furan in processed foods. The analytical method used to analyse furan levels in foods was optimized based on solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS). In baby soups, the concentration of furan decreased by up to 22% after opening a lid for 10 min. In the baby food in retort packaging, the level of furan was reduced by 15–33% after heating the foods at 50°C without a lid. Furan in rice seasonings was evaporated completely after heating the foods at 60°C. Regarding powered milk, the levels of furan were too low to be compared under various conditions. The levels of furan decreased to 58% in beverage products for babies, after storing them at 4°C for 1 day without a lid. The levels of furan in canned foods such as cereal and vegetable were reduced by zero to 52% when they were stored without stirring in a refrigerator at 4°C for 1 day. When we boiled canned fish, the furan present was almost completely evaporated. It is recommended that canned meats be heated up to 50–70°C for the reduction (26–46%) of furan levels. The levels of furan in instant and brewed coffee samples were significantly reduced after storing for 11 to 20 min at room temperature without a lid (p < 0.05).     

固相微萃取-气相色谱-质谱法测定食品塑料包装袋中6 种酞酸酯类化合物

建立固相微萃取-气相色谱-质谱同时测定食品塑料包装袋中6 种酞酸酯类化合物的分析方法,并对固相微萃取方式、萃取溶剂、萃取头涂层、萃取温度等参数进行优化。采用85 μm PA固相微萃取纤维头、正己烷为萃取溶剂,90 ℃平衡5 min后萃取吸附30 min,在250 ℃进样口解吸5 min后供气相色谱-质谱分析。结果表明：该方法的线性范围为0.25～50 mg/L,方法检出限为0.049～0.920 mg/L,回收率为82.2%～109.0%,相对标准偏差（n=6）为4.0%～12.0%,该方法能很好地富集基体中的目标化合物,满足食品塑料包装袋中多种酞酸酯类化合物的分析要求。     

4种主要柑橘类香气成分比较

为探明不同柑橘品种果实的香气成分,采用顶空固相微萃取结合气相色谱-质谱联用法分别对芦柑、脐橙、砂糖橘和狮头柑4个具有典型气味的柑橘品种果皮中的香气成分进行分析,分别从这4个品种果皮样品中检测出挥发性成分39、37、43种和41种,在芦柑和砂糖橘香气中缺少酯类物质,在脐橙香气中缺少酮类物质,狮头柑香气中包括了烃类、醛类、酮类、醇类、酯类、芳香族化合物和一些其他成分,初步从香气成分种类差异、共有香气成分相对含量差异以及各自特有成分上解释了4种果品的香气区别,从化学角度说明了4个柑橘品种果实香气类型的差异。     

固相微萃取-气相色谱-质谱分析青钱柳叶挥发性成分

采用固相微萃取（SPME）和气相色谱-三重串联四极杆质谱联用仪（GC-QQQ-MS）相结合的方法对两个产地（江西修水野生和浙江文成人工栽培）的青钱柳叶挥发性成分进行研究,并比较了它们在挥发性化学成分及含量上的差异。结果表明:在两个产地的青钱柳叶中共鉴定出91种挥发性成分,其中两者共有挥发性成分45种,且主要是碳氢化合物类、醇类、醛类、酯类、酮类、醚类和萘类化合物,但两个样品在挥发性成分的具体组成和含量上存在一定的差异。野生青钱柳叶的挥发性成分主要是β-瑟林烯（18.52%）、石竹烯（8.11%）、β-甜没药烯（6.01%）、β-榄香烯（5.36%）、顺-香叶基丙酮（4.02%）等,人工栽培青钱柳叶的挥发性成分主要是β-波旁烯（11.05%）、β-瑟林烯（10.91%）、石竹烯（7.03%）、苯甲醇（7.01%）、2,6-二甲基-6-（4-甲基-3-戊烯基）-双环[3.1.1]庚-2-烯（5.36%）、2,6,11-三甲基十二烷（5.16%）等。      

基于不同发酵方法制作的曲拉中挥发性风味物质分析

采用顶空-固相微萃取（HS-SPME）方法对传统自然发酵的曲拉与商品发酵剂制作的曲拉样品进行预处理,利用气相色谱-质谱法（GC-MS）检测样品中的挥发性风味成分。经NIST14质谱数据库检索结合文献对照,从传统自然发酵的曲拉中检出29种挥发性风味成分,商品发酵剂制作的曲拉中检出53种,这些挥发性成分中主要包括酸类、醇类、酮类、醛类、酯类、烃类、芳香类。不同发酵方法制作的曲拉中风味物质的种类及含量都存在一定的差异性,这也是使用相同原料不同发酵方法制作的曲拉产生特别的风味的主要原因。      

微波干燥对油菜籽品质及气味成分的影响

利用不同的微波功率将菜籽干燥至安全水分8%,测定干燥后菜籽发芽势、发芽率、油的酸值和过氧化值,并使用固相微萃取-气质联用仪分析菜籽挥发性成分。结果表明:微波功率越高,干燥速率越大;高功率的微波对菜籽的生命力有显著的破坏作用;在110～1 480 W微波功率范围内,菜籽油的酸值变化在合理范围之内,过氧化值在1 170 W功率干燥后呈显著上升趋势;微波功率的增加会导致硫甙分解有害产物的相对含量增加。菜籽的挥发性气体成分中含有硫甙分解生成物、烃类、醛类、酯类、醇类、杂环类、酮类等,其相对含量依次降低。     

顶空固相微萃取-气相色谱-质谱法测定大曲中的土臭素

土臭素（geosmin,GSM）是引起白酒土霉味的一种主要化合物,是在大曲制造过程中由微生物产生的。本文建立了一种简便、快速的顶空固相微萃取气相色谱质谱法（HS-SPME-GC-MS）测定大曲中GSM。大曲样品采用乙醇水溶液进行提取,蒸馏后经HS-SPME处理,GC-MS进行分析,外标法定量。在100⁸000ng/kg的质量浓度范围内,GSM有较好的线性关系,相关系数（r）大于0.99。通过对大曲空白样品进行加标回收率实验和精密度实验考察方法的可行性。结果表明GSM的回收率为89.19%⁹8.49%,相对标准偏差介于2.15%与3.06%之间。GSM的检出限为42.6ng/kg,定量限为140.6ng/kg。本方法适用于大曲中GSM的检测。      

紫花芒果实香气成分的GC-MS分析

使用75μm Carboxen/PDMS和100μm聚二甲基硅氧烷(polydimethylsiloxane,PDMS)两种萃取头提取紫花芒果成熟时果肉和果皮的香气成分,并用气质联用仪定性定量分析香气成分。使用75μmCAR/PDMS萃取头检出果皮香气成分26种,占总挥发物的98.71%,萜类成分占98.49%,挥发性成分相对含量较高的是萜品油烯(44.20%);果肉香气检出21种挥发物,占总挥发物的99.29%,其中萜类占97.82%,相对含量较高的是对伞花烃(55.45%)。使用100μmPDMS萃取头检出果皮香气中22种挥发物,占总挥发物的98.51%,萜类成分占98.14%,其中相对含量较高的是萜品油烯(68.45%);果肉香气中检出15种挥发性成分,占总挥发物的97.68%,萜类占96.69%,相对含量较高的是萜品油烯(79.18%)。紫花芒果更适合使用75μmCarboxen/PDMS提取香气成分进行分析,且果皮中的香气成分多于果肉中,主要是萜类成分。     

固相微萃与GC/MS联用分析水蜜桃挥发性成分

采用固相微萃取技术萃取新鲜和腐败的水蜜桃挥发性成分,并通过气相色谱质谱联用法来分析、鉴定水蜜桃中的气味成分。经NIST质谱数据库检索和文献对照,新鲜水蜜桃检测出32种成分,占总峰面积的81.48%;腐败的水蜜桃检测出27种成分,占总峰面积的86.56%。相同成分有辛酸乙酯、4-癸酸乙酯、辛酸己酯、1,2-苯二羧基酸丁辛酯、异丙基棕榈酸酯、4-(2,6,6-三甲基)-2-丁酮、5-乙二氢基-2(3H)呋喃酮、十五烷、十六烷、十七烷等20种物质,但其相对含量存在很大差异。结果表现出水蜜桃不同品质果实气味成分的不同,可应用于果实的质量鉴定。     

Preliminary assessment of the risk linked to furan ingestion by babies consuming only ready-to-eat food

The risk linked to furan ingestion has been assessed in previous papers for Belgian adults and children. The present paper focuses on infants consuming only ready-to-eat baby food. As there is no Belgian baby dietary database, the furan exposure assessment was carried out by using an Italian infant consumption database and Belgian contamination data. The estimated daily intake (EDI) was calculated according to a deterministic methodology. It involved 42 commercially available ready-to-eat baby food and 36 baby consumption records. The mean EDI was 1460 ng*(kg_bw*day)^?1 which is 3.8 times higher than the 381 ng*(kg_bw*day)^?1 reported for Belgian adults, and 3.5 times higher than the 419 ng*(kg_bw*day)^?1 measured for Belgian children. To assess and characterise the risk for babies’ exposure, the margin of exposure (MoE) was calculated. It highlighted that 74% of infants have a MoE < 1000, with a minimum of 140. However, these are only preliminary results as they were calculated from a very small dataset and the infant cytochrome P450 activity is significantly different compared with the adult’s. Therefore, the risk linked to furan ingestion by babies should be assessed in a different manner. To this end, additional data regarding a baby diet as well as a better understanding of furan toxicity for babies are needed to characterise more accurately the risk for infants.     

气相色谱-质谱法中4种不同捕集方式对茶叶香气成分测定的影响

采用固相微萃取(solid phase microextraction,SPME)、吹扫捕集-热脱附(purge & trap-thermal desorption,P&T-TD)、搅拌磁子吸附(stir bar sorptive extraction,SBSE)、动态顶空吸附(head space sorptive extraction,HSSE-1、HSSE-2和HSSE-3)4种捕集方式联用气相色谱-质谱仪对杭州龙井茶、黄山毛峰茶、山东崂山茶和福建乌龙茶进行分析,研究茶的挥发性香气组分。结果显示：茶的香气主要由烯类、醛类、醇类、酮类、酯类、酸类、芳香族化合物、含氮化合物、杂环化合物、含硫化合物、酚类化合物组成;4类茶均含有大量的烯类、醛类、醇类和酮类化合物,其中福建乌龙茶含量最高;杭州龙井茶、黄山毛峰茶和山东崂山茶属绿茶类,酯类、杂环类、芳香族类以及酚类化合物含量相对较高;通过HSSE-1、HSSE-2对茶叶香气成分进行对比,冲泡前后组分种类和含量略有不同。组分之间的差异使茶形成不同产地不同种类的茶叶的特有风味。     

不同解冻时间对冰鲜牡蛎挥发性风味物质的影响

采用固相微萃取法提取,利用气相色谱-质谱法对冰鲜牡蛎中挥发性物质进行分离鉴定。结果表明,利用该方法鉴定出的冰鲜牡蛎的挥发性物质共有39种,主要挥发性物质有己醛、1-辛烯-3-醇、3-辛酮等;进一步研究不同解冻时间,挥发性物质的种类和相对含量的变化表明,随着解冻时间的延长,挥发性物质中醛酮类相对含量减少,胺类相对含量增加,其他化合物也增多。     

Polycyclic aromatic hydrocarbon levels and risk assessment for food from service facilities in Korea

ABSTRACT

In this study, levels of benzo[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene (BaP), dibenzo[a,h]anthracene, benzo[g,h,i]perylene and indeno[1,2,3-c,d]pyrene in 412 food items collected from food service facilities in Korea were analysed. The concentrations of the eight polycyclic aromatic hydrocarbons (PAHs) ranged 0.13–0.48 μg/kg. The concentrations of benzo[a]pyrene in all food samples were <1 μg/kg, which is the lowest maximum limit in foods regulated by European Union legislation. PAH contents were employed to conduct exposure and risk assessment. The chronic daily intake of PAHs from 412 food samples was 5.48 × 10^–6-4.70 ×x 10^–4 µg-TEQ_BaP/kg/day with margins of exposure of 1.04 × 10⁹-1.16 × 10¹¹.     

曲霉型豆豉后发酵过程中挥发性成分的动态变化

运用固相微萃取气-质联用技术对曲霉型豆豉后发酵过程中不同时期的挥发性成分进行分析,用面积归一化法测定其组分的相对含量,通过主成分分析法对其相对含量进行分析,鉴定出的整个后发酵过程中主要挥发性风味物质包括醇类5种、酯类7种、醛类3种、酸类1种、酮类1种、吡嗪类1种、烷烃类2种,共20种。随着后酵的进行,检测出的挥发性成分种类逐渐增加,其中1-辛烯-3-醇、3-甲基丁醇、2-甲基丁酸乙酯、己酸乙酯、苯乙醛、3-乙氧基丙烯、4-羟基2-丁酮、4-甲基吡嗪和2-甲基-丙酸乙酯为豆豉整个后发酵过程中主要的挥发性风味物质。而3-甲基丁醇、2-甲基丁酸乙酯、己酸乙酯、4-甲基吡嗪和2-甲基-丙酸乙酯则对豆豉后酵过程中风味形成贡献较大,且其含量随着后酵进行逐渐增加。同时,通过主成分分析得出,在整个后酵过程中15d时,样品的风味最好,25d和30d次之。     

固相微萃取-气相色谱质谱联用分析花椒挥发性成分

研究不同加工方式下花椒香气的变化。以陕西韩城市产花椒为原料,利用固相微萃取-气相色谱质谱联用技术分析焙烤花椒和风干花椒中的挥发性成分。结果从焙烤花椒中共鉴定出48种挥发性成分,其中主要挥发性成分为α-蒎烯(4.14%)、6,6-二甲基-2-亚甲基-双环[3.1.1]庚烷(5.63%)、1-甲基-4-(1-甲乙基)-1,4-环己二烯(3.20%)、1,7,7-三甲基-三环[2.2.1.0(2,6)]庚烷(6.96%)、β-水芹烯(9.47%)、甲酸(8.50%)、3-蒈烯(3.62%)、3,7-二甲基-1,6-辛二烯-3-醇(3.09%)、4-甲基-1-(1-甲乙基)-3-环己烯-1-醇(5.34%)、α,α,4-三甲基-3-环己烯-1-甲醇(6.12%)、α-异戊酸松油酯(8.91%)、1,2,4α,5,8,8α-六氢-4,7-二甲基-1-(1-甲乙基)-萘(4.32%)、1-甲基-5-亚甲基-8-(1-甲乙基)-1,6-环癸二烯(5.07%);从风干花椒中共鉴定出49种挥发性成分,其中主要挥发性成分为α-蒎烯(3.38%)、6,6-二甲基-2-亚甲基-双环[3.1.1]庚烷(9.38%)、1-甲基-4-(1-甲乙基)-1,4-环己二烯(14.74%)、2-甲基-5-(1-甲乙基)-双环[3.1.0]己-2-醇(3.00%)、1,7,7-三甲基-三环[2.2.1.0(2,6)]庚烷(18.45%)、β-水芹烯(9.80%)、3,7,7-三甲基-双环[4.1.0]庚-3-烯(10.89%)、2,6-二甲基-2,4,6-辛三烯(3.37%)、3-蒈烯(3.11%)、cis-β-松油醇(5.30%)。焙烤花椒和风干花椒的挥发性成分有较大差别。     

外源添加物对酱油发酵的影响

研究不同酱油的香气差异有利于从原料和酿造工艺角度加强其风味品质控制和质量提升。采用固相微萃取和固相萃取与气相色谱-质谱联用法对10种特级酱油（CB、HT1、HT2、LH、LJJ1、LJJ2、QH、XH1、XH2、WZ）中的挥发性香气成分进行定性和定量分析,结合感官评价、香气活性值（Odor activity value,OAV）和偏最小二乘回归分析（Partial least squares regression,PLSR）进一步分析不同特级酱油的香气差异及其贡献。结果表明,在10种特级酱油中共检测到86种香气化合物,其中44种化合物在10种酱油中共有。共30种香气物质的OAV ≥1,其中5-乙基-4-羟基-2-甲基-3（2H）-呋喃酮的OAV（373~4698）值最高,其次为4-甲氧基-2,5-二甲基-3（2H）-呋喃酮（0~1473）。WZ酱油的烟熏香较强,其酚类和酮类化合物种类最多。CB酱油整体香气强度最小,乙醇（25.775 μg/L）远低于其余9种酱油;但其吡嗪类物质含量最高（182.796 μg/L）,其中2,6-二甲基吡嗪含量为66.256 μg/L。XH1酱油的酱香与醇香较为强烈,其乙醇（147.257 μg/L）含量最高,酚类物含量同样较高,其中4-乙基-2-甲氧基苯酚为18240.479 μg/L。XH2酱油的麦芽香强烈。LH酱油的异丁醇（51.223 μg/L）和2,3-丁二醇（57921.798 μg/L）含量在所检测样品中均为最高。HT1酱油中1-辛烯-3-醇（61.219 μg/L）含量最高。综合OAV与PLSR分析,乙酸乙酯、3-羟基-2-丁酮、2,3-丁二醇、3-乙基-2,5-二甲基吡嗪、4-甲氧基-2,5-二甲基-3(2H)-呋喃酮、4-乙基愈创木酚和4-乙基苯酚为10种特级酱油香气差异的关键成分。

     

婴儿奶瓶及食品包装材料中双酚A的风险评估

双酚A作为婴儿奶瓶及食品包装材料的生产原料是否对人类的健康有潜在风险以及风险的大小如何,是公众和政府密切关注的问题.根据风险评估理论的四个步骤,即危害鉴定、危害特征描述、暴露评估和风险特征描述,对双酚A进行风险评估,结果表明人体暴露于双酚A的量是微不足道的,没有对人体健康构成已知的风险.