Determination of the overall migration from silicone baking moulds into simulants and food using 1H-NMR techniques

Different silicone baking moulds (37 samples) were characterized with respect to potential migrating substances using ¹H-NMR, RP-HPLC–UV/ELSD and GC techniques. In all cases cyclic organosiloxane oligomers with the formula [Si(CH₃)₂–O] _n were identified (n = 6 … 50). Additionally, linear, partly hydroxyl-terminated organosiloxanes HO–[Si(CH₃)₂–O] _n –H (n = 7 … 20) were found in 13 samples. No substances other than siloxanes could be detected, meaning the migrants mainly consist of organopolysiloxanes. Based on this knowledge, a ¹H-NMR quantification method for siloxanes was established for the analysis of both simulants and foodstuffs. Validation of the ¹H-NMR method gave suitable performance characteristics: limit of detection 8.7 mg kg^–1 oil, coefficient of variation 7.8% (at a level of 1.0 mg kg^–1 food). Migration studies were carried out with simulants (olive oil, isooctane, ethanol (95%), Tenax) as well as preparation of different cakes. From the 1st to 10th experiment, siloxane migration into cakes only slightly decreased, with a significant dependence on fat content. Migration never exceeded a level of 21 mg kg^–1 (3 mg dm^–2) and was, therefore, well below the overall migration limit of 60 mg kg^–1 (10 mg dm^–2). However, migration behaviour into simulants differed completely from these results.     

Relationship between physicochemical properties and maximum residue levels and tolerances of crop-protection products for crops set by the USA, European Union and Codex

Residues on foodstuffs resulting from the use of crop-protection products are a function of many factors, e.g. environmental conditions, dissipation and application rate, some of which are linked to the physicochemical properties of the active ingredients. Residue limits (maximum residue levels (MRLs) and tolerances) of fungicides, herbicides and insecticides set by different regulatory authorities are compared, and the relationship between physicochemical properties of the active ingredients and residue limits are explored. This was carried out using simple summary statistics and artificial neural networks. US tolerances tended to be higher than European Union MRLs. Generally, fungicides had the highest residue limits followed by insecticides and herbicides. Physicochemical properties (e.g. aromatic proportion, non-carbon proportion and water solubility) and crop type explained up to 50% of the variation in residue limits. This suggests that physicochemical properties of the active ingredients may control important aspects of the processes leading to residues.     

Emulsifying properties of protein–pectin complexes and their use in oil-containing foodstuffs

The emulsifying properties of proteins have been well studied as they are important for the preparation of creams, mayonnaises and other oil/fat-containing foodstuffs. The emulsifying action of a protein is not always sufficient to obtain stable emulsions of good quality. The use of chemical stabilisers in the food industry is not desirable. One of the best ways to improve the quality of emulsions and to produce emulsions with high nutritive value is to use protein-polysaccharide complexes as emulsifiers. Varying the protein-polysaccharide ratio in the complex, and also the kind of the polymers, would vary the quality and the nutritional value of the foodstuff. Four non-conventional protein preparations were tested as emulsifiers and their emulsifying properties were improved by the addition of pectin. This makes it possible to create new foodstuffs with low oil content and high nutritional value.     

Presence of CP4-EPSPS Component in Roundup Ready Soybean-Derived Food Products

With the widespread use of Roundup Ready soya (event 40-3-2) (RRS), the traceability of transgenic components, especially protein residues, in different soya-related foodstuffs has become an important issue. In this report, transgenic components in commercial soya (including RRS) protein concentrates were firstly detected by using polymerase chain reaction (PCR) and western blot. The results illustrated the different degradation patterns of the cp4-epsps gene and corresponding protein in RRS-derived protein concentrates. Furthermore, western blot was applied to investigate the single factor of food processing and the matrix on the disintegration of CP4-EPSPS protein in RRS powder and soya-derived foodstuffs, and trace the degradation patterns during the food production chain. Our results suggested that the exogenous full length of CP4-EPSPS protein in RRS powder was distinctively sensitive to various heat treatments, including heat, microwave and autoclave (especially), and only one degradation fragment (23.4 kD) of CP4-EPSPS protein was apparently observed when autoclaving was applied. By tracing the protein degradation during RRS-related products, including tofu, tou-kan, and bean curd sheets, however, four degradation fragments (42.9, 38.2, 32.2 and 23.4 kD) were displayed, suggesting that both boiling and bittern adding procedures might have extensive effects on CP4-EPSPS protein degradation. Our results thus confirmed that the distinctive residues of the CP4-EPSPS component could be traced in RRS-related foodstuffs.     

Supramolecular solvent-based microextraction of Sudan dyes in chilli-containing foodstuffs prior to their liquid chromatography-photodiode array determination

A supramolecular solvent made up of reverse micelles of decanoic acid was proposed for the simple and rapid extraction of Sudan I, II, III and IV from chilli-containing foodstuffs. The procedure involved the extraction of minute quantities (0.5–1 g) of homogenised food sample with an aqueous solution containing 10% THF and 200 mg of decanoic acid, conditions under which the supramolecular solvent (around 330 μL) formed in situ and instantaneously. The overall sample treatment took about 30 min and several samples could be simultaneously treated using conventional lab equipment. No clean-up or solvent evaporation were required before determination of Sudan dyes by liquid chromatography and photometric detection. Extractions were independent of salt addition (up to 1 M), the temperature (up to 60 °C) and the pH (below 4) rendering the method robust. The detection limits of the method were 4.2, 2.7, 6.5 and 7.4 μg kg⁻¹ for Sudan I, II, III and IV, respectively. Recoveries obtained by applying this approach to the analysis of six chilli-containing sauces fortified with Sudan dyes at the μg kg⁻¹ level were in the interval 86–108% with relative standard deviations between 2% and 7%.     

特异性定量测定油脂和含油食品酸价的新铜皂比色法

建立了一种可特异性测定食用油脂及含油食品中游离脂肪酸（FFA）的新铜皂比色法。优化了铜皂比色法的最佳测定波长,研究了有机相溶剂对显色强度和油脂溶解稳定性的影响,以及不同种类FFA对铜皂反应显色强度的影响。此外,研究了食用油脂样液水洗、酸性食品添加剂和酸性食用香精香料对铜皂比色法测定的影响。结果表明：新铜皂比色法的最佳测定波长为710 nm,环己烷是理想的有机相溶剂;新铜皂比色法能有效排除酸性食品添加剂等非FFA的酸性物质干扰;该法采用油酸显色,外标法定量,可实现0.1~5.0 mg/g的液态油和0.2~10.0 mg/g的固态脂酸价的定量测定;对于无酸性物干扰的食用油脂,其测定结果与传统酸碱滴定法相关性良好（R2>0996）,回收率为91.3%~93.8%,重复性实验相对标准偏差小于3%,单次测定仅需1 g油脂样品。因此,新铜皂比色法是一种准确而便捷的酸价测定技术,适用于油脂和含油食品的酸价测定。     

高效液相色谱-串联质谱法测定植物源食品中特丁硫磷、特丁硫磷砜和特丁硫磷亚砜的残留量

目的建立高效液相色谱-串联质谱法测定植物源食品中特丁硫磷、特丁硫磷砜和特丁硫磷亚砜残留量的分析方法。方法样品采用乙腈或1%乙酸-乙腈提取,提取液经分散固相萃取净化。以CORTECSC18(100 mm×2.1 mm, 2.7mm)色谱柱分离待测物,以0.1%乙酸铵甲醇溶液和0.1%甲酸加乙酸铵水溶液为流动相,梯度洗脱,流速为0.3m L/min,柱温35℃。目标化合物采用电喷雾正离子电离、多反应监测模式检测,以基质匹配校准曲线外标法进行定量分析。结果 3种化合物的相关系数均大于0.997, 3种化合物的检测定量限均低于0.005 mg/kg。3种化合物在10种基质(柑橘、苹果、大葱、黄瓜、西兰花、菠菜、胡萝卜、花生、大米、茶叶)中3个添加水平(0.005、0.01、0.05 mg/kg)的回收率为79.2%~105%,相对标准偏差为1.2%~20.1%。结论该方法简便、灵敏、环保,回收率和精密度好,适合于植物源食品中特丁硫磷及其氧类似物(砜、亚砜)残留的检测。     

催化动力学分光光度法测定食品中的硒含量

本文对在酸性介质中Se（IV）强烈催化H2O2氧化二甲基黄的褪色反应进行了一系列的研究，拟定了用催化动力学分光光度法测定Se（IV）的最佳条件及测定方法。     

食品中全氟化合物分析技术研究进展

全氟化合物(perfluorinated compounds,PFCs)是一类人工合成的脂肪烃类化合物,自上个世纪50年代合成以来,该类化合物以其优良的稳定性及表面活性作为加工助剂被应用于多种民用及工业领域,如纺织品、灭火器和油漆等行业。近些年来越来越多的调查研究发现,在空气、沉积物、饮用水、海水和食品中检测出全氟类化合物。膳食作为人体暴露PFCs的重要途径之一,已受到了各国研究人员的重视。本文综述了食品中PFCs的检测技术的研究进展,讨论了不同食品中PFCs的前处理及检测方法,当前主要采用离子对液液萃取和液固萃取,WAX柱净化提取液,液相色谱-质谱联用技术定量分析食品中的PFCs。由于食品中PFCs处于痕量水平,对该类物质的检测方法中空白本底的控制尤为重要。另外,全氟化合物存在的多种同分异构体之间的差异将是研究人员对其准确监测的困难之一。     

高温加热食品丙烯酰胺问题的探讨

丙烯酰胺对人和动物是一种有效累积性神经毒物，近年来研究发现在高温加热食品中有丙烯酰胺产生，本文介绍了高温加热食品中丙烯酰胺的形成机理、影响其形成的各种因素以及测定其含量的各种方法，最后提出了降低丙烯酰胺的一些措施．