纸质包装材料中甲醛、乙醛向食品模拟物改性聚苯醚的迁移行为

为了解纸质包装材料中甲醛、乙醛向食品模拟物改性聚苯醚( Tenax)中的迁移行为,建立了一步提取衍生化、超高效液相色谱测定纸质包装材料和Tenax中的甲醛和乙醛的方法。本方法在甲醛和乙醛的测定范围内,线性相关系数R2>0.9999,甲醛检出限为0.03 mg/m2,乙醛检出限为0.04 mg/m2,测定纸样和Tenax的加标回收率为90.1%~108.6%。采用本方法研究不同温度和时间下两种纸质包装材料中甲醛、乙醛向Tenax中的迁移规律。研究表明,甲醛、乙醛迁移行为随时间变化趋势大致相同,均呈现迁移率随迁移时间延长先迅速增大,后又减小达到一个常数;甲醛和乙醛迁移率受温度的影响不同,达到平衡后,甲醛在30℃下迁移率最高,乙醛在70℃和50℃下迁移率高;甲醛和乙醛向Tenax中的迁移率差异较大,达到平衡后,乙醛的迁移率远高于甲醛。     

纸基包装材料中抗氧化剂及增塑剂向干性食品模拟物Tenax TA迁移的研究

采用改性聚苯醚多孔聚合物微球Tenax TA为干性食品模拟物,用于纤维素纸基食品接触材料中3-叔丁基-4-羟基苯甲醚(BHA)、2,6-二叔丁基-4-甲基苯酚(BHT)和邻苯二甲酸二环己酯(DCP)向Tenax TA迁移的研究,以超高效液相色谱进行测定。迁移试验以白卡纸和牛皮纸为研究对象,通过设计不同迁移时间和迁移温度下3种目标物向Tenax TA迁移的实验,获取有机化合物从纸基纤维素向Tenax TA迁移的规律。结果表明,有机化合物从纸基材料向多孔聚合物微球的迁移经历了气体吸附和脱附两个步骤。在Tenax TA吸附目标化合物的过程中,纤维素纸基材料的微观孔径尺寸越大,与迁移物的相互作用越小,迁移物迁移的速率越大,Tenax TA的吸附效率越高;当吸附达到平衡后,迁移时间的延长会引发Tenax TA中迁移物的脱附,进而导致目标化合物的迁移率下降。对45种纸基食品接触材料中目标迁移物的筛查表明,BHA和DCP分别存在于两种不同类型的纸基食品接触材料中,迁移量分别为0.027μg/dm~2和0.81μg/dm~2,均小于欧盟指令规定的特定迁移限量。     

Characterization of poly(2,6-diphenyl-p-phenylene oxide) films as adsorbent for microfabricated preconcentrators

This work aims at evaluating poly(2,6-diphenyl-p-phenylene oxide) (Tenax TA), in the form of thin films, as an adsorbent material for various analytical applications. The physical properties of the polymer were studied with regard to surface topography, crystal structure, and thermal stability. Films deposited from solution at different substrate temperatures were studied and compared to the granular form of the polymer. It was found that Tenax TA deposited from solution have a different topography compared to their granular counterpart. The films possess a complex phase composition that includes crystalline and amorphous phases. The films showed high thermal stability (400 °C) similar to the granular form. The adsorption performance of the polymer compared to other possible adsorbent films such as polydimethylsiloxane (PDMS) and layer-by-layer assembled gold nanoparticles (GNPs) were also investigated. Representative volatile organic compound samples were used to compare the adsorption properties of Tenax TA films to that of the granules.     

Headspace methods for volatile components of grapefruit juice

Summary Static headspace, dynamic headspace (DHS) and strip/trap methods were evaluated with grapefruit juice volatiles and an aqueous model system of selected grapefruit volatile flavour components, to select the best method for the isolation of volatile components for subsequent GC analysis.Recoveries were calculated for these methods in the concentration range 0.01–10gml^–1 and compared. Analyte trapping followed by thermal desorption was performed with Tenax TA traps which gave good results in terms of very low blanks. DHS analysis gave the best results in terms of recovery efficiency and, if adequately combined with a simultaneous steam distillation/solvent extraction method, is the most suitable for the qualitative and quantitative investigation of grapefruit juice volatiles, and it might be extended to other fruit juices or liquid foods.     

气提浓缩仪分析水中痕量挥发性有机物研究

本文描述了气提浓缩仪的设计及操作程序用于对水中痕量挥发性有机物的测定。分析物被气提吸附于TenaxGC柱上,然后直接脱附到毛细管气相色谱柱上进行分析,并用FID或MS鉴定。本文除对色谱条件进行优化外,对气提时间和脱附温度等分析操作条件也进行了研究。检测下限为0.01-0.30PPb,峰面积检测精度优于6.9％,对16种化合物的回收率优于74％。     

Determination of beer aroma compounds using headspace solid-phase microcolumn extraction

A rapid sampling technique for the analysis of beer aroma compounds is described. The headspace (10 ml) is passed through the microcolumn filled with 5 mg of Tenax TA and thermally desorbed in a modified GC inlet (modification is described). Eight compounds (from acetaldehyde to 2-phenylethanol) in four beer samples were analyzed. The correlation coefficients (r²), repeatability (RSD) and limits of detection (LOD) were 0.9973-0.9994, 2.1-6.9% and 0.00002-0.13 mg/l, respectively. The methodology can be useful for routine beer sample analysis.     

Novel multi-sorbent for sampling and determination of trace volatile organic sulfur compounds in ambient air

Novel adsorbent APSG-MW (average particle size 215?µm and specific surface 98 m²?g^?1) bonding multi-walled carbon nanotubes (MWCNTs) on silica gel are obtained. Then the sampling tubes filled with Tenax TA and APSG-MW are prepared and the adsorptive capacity of Tenax TA/APSG-MW for volatile organic sulfur compounds (VOSCs) is studied. The data show that the adsorption and desorption recoveries of multi-sorbent for VOSCs are satisfactory (>85%), and the breakthrough values are large (>16?L?g^?1) enough to absorb VOSCs in ambient air. The sampling precision of the sorbent tubes meets TO-17 criteria. The sampling tubes are successfully used to concentrate and analyze a sample of landfill air, and the major S compounds are identified.     

A new sensitive alternative of static headspace gas analysis with sample-addition calibration

Summary A method is described which makes it possible to with-draw in a defined way headspace gas samples amounting to as much as several tens of milliliters from an equilibrated gas-liquid system. The apparatus consists of an equilibration vessel provided with a septum through which a Tenax GC-packed trap can be connected with the headspace compartment via an injection needle. At the bottom of the vessel, a syringe is situated by means of which a liquid sample is introduced into the vessel. A portion of liquid sample is introduced into the equilibration vessel, equilibrium is established, a certain volume of the headspace gas is pushed out through the trap by introducing another portion of liquid sample, and the analytes entrapped are determined by GC. Then the entire procedure is repeated, and the initial contents of the analytes in the liquid sample are calculated from the two GC analyses. The possibilities and reliability of the method are discussed.Presented at the 14th International Symposium on Chromatography London, September, 1982     

Needle‐trap device for the sampling and determination of chlorinated volatile compounds

A needle‐trap device, with immobilized sorbent inside the syringe, coupled with GC–MS was applied for air sampling and determination of chlorinated volatile organic compounds such as dichloromethane, trichloromethane, and tetrachloromethane. The application of a needle trap packed with combination of three sorbents including Tenax TA, Carbopack X, and Carboxen 1000 resulted in detection limits of few pg for chlorinated volatile compounds and recoveries of 99.2–102.8%. The extraction and desorption parameters were optimized within the study. As a result, the precision determined as RSD was equal to 5.05 and 3.03 and 6.52% for dichloromethane, trichloromethane, and tetrachloromethane, respectively. The storage time for chlorinated compounds up to 48 h and reusability of the needle‐trap device were verified. The obtained results have proved the ability of needle traps to compete with other solventless sampling and sample preparation extraction techniques.