Pd/Ce0.6Zr0.4O2/Al2O3 as advanced materials for three-way catalysts: Part 1. Catalyst characterisation, thermal stability and catalytic activity in the reduction of NO by CO

Pd-loaded Ce_0.6Zr_0.4O₂ solid solutions supported on Al₂O₃ are investigated as catalysts for the reduction of NO by CO. The attention is focused on the role of the Ce_0.6Zr_0.4O₂ and of the Pd dispersion on the catalytic activity. The system shows a very high activity below 500 K, which is almost independent on the Pd dispersion. The high activity is attributed to a promoting effect of the Ce_0.6Zr_0.4O₂ on the NO conversion. Investigation of the influence of high temperature treatments disclosed a thermal stabilisation of both Ce_0.6Zr_0.4O₂ and Al₂O₃ in the Ce_0.6Zr_0.4O₂/Al₂O₃ system.     

固相微萃取法分析凤凰单枞乌龙茶香气组分

本文以凤凰单枞乌龙茶（Camellia sinensis）为材料，采用固相微萃取（solid Phase Microextraction，SPME）对其呈香组分进行研究。结果表明采用SPME萃取凤凰单枞乌龙茶香气组分，从桂花香型乌龙茶干茶样中检测出41种香气组分，而SDE法则检测到55种香气组分，两种方法都检测出高比例的芳樟醇、橙花叔醇、茉莉酸甲酯和吲哚。SPME法萃取了乌龙茶自身散发出的香气组分，避免了茶叶中易挥发或热不稳定的香气组分被破坏，减少了香气组分的测定误差和不稳定性。     

Determination of Trace Para Red Residues in Foods through On-Line Molecularly Imprinted Solid Phase Extraction Coupled with High-Performance Liquid Chromatography

ABSTRACT:  In this article, we prepared a novel imprinted polymer by a room temperature ionic liquid-mediated surface molecular imprinting technique in combination with a sol–gel process. This polymer was characterized by static and kinetic adsorption experiments and exhibited good recognition ability and offered fast kinetics for the adsorption of Para Red. A simple and sensitive analytical method, based on the coupling of molecularly imprinted solid phase extraction with high-performance liquid chromatography (HPLC), had been developed for determination of trace Para Red. With a loading flow rate of 0.42 mL min⁻¹ for 25 mL, an enrichment factor of 1061 was achieved. Under the selected experimental condition, the detection limit (S/N = 3) of Para Red was 6.6 ng L⁻¹, and the peak area precision (RSD) for 5 replicate detections of 0.15 μg L⁻¹ Para Red was 4.1%. The applicability of this method for determination of the blank chili sauce sample, spiked with Para Red at 5 to 25 ng g⁻¹ levels, was demonstrated, with recoveries ranging from 86% to 95%.
Practical Application: In this paper, a simple and sensitive analytical method, based on the coupling of molecularly imprinted solid phase extraction with high performance liquid chromatography, had been developed for determination of trace Para Red. It was applied to the analysis of spiking Para Red in chili sauce sample with satisfactory recovery and repeatability. This proposed method has the potential to be used for monitoring the illegal addition of Para Red in foods in the future due to its simple, reliable, rapid, and excellent precision.     

高能固体推进剂化学安定性研究(Ⅰ)——热失重影响因素的研究

研究了NEPE高能固体推进剂在不同贮存条件下的热失重行为,得出了样品贮存条件与热失重有如下关系:当样品尺寸和贮存条件相同时,随温度升高,高能固体推进剂热失重率增大。当样品尺寸和温度相同时,贮存在敞开条件下的样品热失重率显著大于密闭贮存条件。比较敞开条件与密闭条件贮存时硝酸酯含量随时间的变化后认为,高能固体推进剂在敞开和密闭条件下热失重率的差异与硝酸酯挥发存在紧密关系。     

Kinetic analysis of non-enzymatic browning in carrot juice concentrate during storage

The effect of storage temperature, storage time and total soluble solid (TSS) on the total sugar (TS), sucrose, glucose, fructose, total amino acid (TAA), pH, 5-hydroxymethylfurfural (HMF) and browning degree (BD) in carrot juice concentrate (CJC) stored at −18, 0, 25 and 37 °C was studied and the relationship between HMF and BD was established. Higher temperature at 25 and 37 °C had a significant effect (p<0.05) on TS, sucrose, glucose, fructose, TAA, pH, HMF and BD, while lower temperature at 0 and −18 °C had less effect, and the storage time and the soluble solid of CJC stored at 25 and 37 °C also had a significant effect on HMF formation and BD. At 25 and 37 °C, the formation of HMF and BD followed a first-order reaction well as a function of storage time; a good correlation between HMF formation and BD occurred. The formation of HMF could described by the total soluble solid value [TSS] and the BD value ([BD], absorbance at 420 nm) of CJC, the equation was [HMF] (content of HMF) = 1.2177 − 0.1124 × [TSS] + (2.835 + 0.3477 × [TSS]) × [BD] and [HMF] = 1.5510 − 0.4813 × [TSS] + (23.8847 + 0.7249 × [TSS]) × [BD] at 25 and 37 °C, respectively.     

分散固相萃取-气相色谱-四极杆-飞行时间质谱法快速测定鲜鱼中的5种酚类麻醉剂

【目的】建立了以分散固相萃取技术为前处理手段,结合气相色谱-四极杆-飞行时间质谱(gas chromatography-quadrupole time of flight mass spectrometry, GC-Q-TOF/MS)测定鲜活鱼中5种酚类麻醉剂的快速分析方法。【方法】样品经乙酸乙酯提取后,氮气浓缩,复溶液使用C18和PSA混合粉末净化,GC-Q-TOF/MS测定。采用电子轰击离子源(electron impact ion source, EI)进行电离,选择离子对模式对目标母离子和子离子进行测定。【结果】5种酚类麻醉剂的基质曲线在5.0~500 μg/L范围内呈良好线性关系,相关系数r²均大于0.999,日内不同水平的加标回收率在3.58%~8.96%之间,相对标准偏差(RSD)为2.56%~5.28%。方法检出限(limits of detection, LOD)为3.58~8.96 μg/kg。【结论】该方法操作简单、回收率好、灵敏度高、重复性好,可满足鲜活鱼中酚类麻醉剂快速测定的要求。     

滑石颜料高剪切流变性能的研究

使用毛细管高剪切黏度仪研究了滑石颜料分散体系的高剪切黏度性能,以及pH值、固含量、不同分散剂和润湿剂、不同粒径分布对滑石分散体系高剪切黏度的影响。同时还研究了滑石与GCC及高岭土混合浆料的高剪切黏度性能。结果表明,滑石含量越高、粒度越细,其分散浆料的高剪切黏度值越大。同时发现,滑石高剪切黏度受分散剂和润湿剂的影响不大。提高pH值有利于降低滑石分散体系的高剪切黏度。滑石与GCC混合浆料的高剪切黏度随着GCC粒度的变细而降低。当滑石与GCC的体系中加入高岭土后,混合浆料的高剪切黏度大幅增大,且随着GCC粒度的变细而增大。     

两种海洋节肢动物风味物质的分析与评价

目的:利用固相微萃取技术分析渤海产地三疣梭子蟹和口虾蛄肌肉中的风味化合物.方法:采用涂有聚二甲基硅氧烷-二乙烯苯(PDMS-DVB)涂层的固相微萃取头萃取挥发性化合物,并通过气相色谱质谱联用来分析鉴定两种海洋节肢动物肌肉中的风味成分.结果:固相微萃取技术有效提取了三疣梭子蟹和口虾蛄肌肉中的呈味物质,经过 NIST 质谱数据库和文献对照,分别确定了20种和15种主要呈味物质,大多是一些酸类、酯类、醛类、醇类等化合物.结论:两种海洋节肢动物所含有的风味物质因其含量及构成比例不同而形成了各自独有的风味和口感.     

固相萃取-气相色谱法测定桑葚等浆果中百菌清、腐霉利和联苯菊酯3种农药残留

目的建立固相萃取-气相色谱法测定桑葚等浆果中百菌清、腐霉利和联苯菊酯3种农药残留的分析方法。方法乙腈提取桑葚浆果样品中的3种农药,提取液经HLB固相萃取柱富集、净化,丙酮+环己烷(1:9,V:V)洗脱,洗脱液氮吹至近干,环己烷定容至1 mL,上气相色谱仪定量检测。结果百菌清、腐霉利和联苯菊酯在浓度为0.002～0.200μg/mL范围内线性关系良好;百菌清、腐霉利和联苯菊酯定量限分别为0.0002、0.0006、0.0006 mg/kg;方法加标回收率在85.8%～99.7%之间;精密度和重复性RSD均在10.0%以内。结论方法具有简便、准确、快速等特点,可以用于桑葚等浆果中的农药残留检测。     

4 种不同品质猪肉香气的差异

为全面了解瘦肉型猪肉、定远黑猪肉、安庆六白猪肉和皖南花猪肉香气的差异,将这4 种新鲜猪肉分别熟制后,采用固相萃取-气相色谱-质谱法分析其挥发性风味成分及含量,计算出相应的香气值,采用主成分分析法分析4 种猪肉香气的差异。结果表明：瘦肉型猪肉香气与其他3 种中国地方猪肉的香气有着明显差异,其余3 种中国地方猪肉的香气也有一定差异;对瘦肉型猪肉与其他地方猪肉香气差异影响较大的香气物质有：柠檬烯、己醛、庚醛、（E）-十四碳烯-1-醇、2-乙基呋喃、2-正戊基呋喃、2-正己基呋喃、十四碳烯-1-醇和庚酮。苯甲醛与皖南花猪肉的香气相关性较高,安庆六白猪肉样品的香气与柠檬烯、十一醛和庚酮的相关性最高,14-十碳烯醛、辛醛、庚醛和（E）-十四碳烯-1-醇与定远黑猪肉样香气联系紧密,没有与瘦肉型猪肉香气相关性较高的挥发性风味物质。