有机硅乳液中挥发性物质的测定

根据固相微萃取原理,对萃取条件进行了优化。优化后的HS-SPME-GC-MS(顶空固相微萃取/气相/质谱)实验条件为:采用85μm PAA纤维萃取头,萃取时间30min,萃取温度室温,解吸时间5min。在此条件下对3种有机硅乳液进行分析,通过计算机数据系统(质谱数据库NIST和Willy)检索及人工谱图解析,鉴定了非硅油挥发性成分。该方法的相对标准偏差为0·57%~2·59%。     

馒头挥发物质的固相微萃取条件优化

以总峰面积和峰数为评价指标,研究了以聚二甲基硅氧烷(DVB/CAR/PDMS)为萃取头的固相微萃取(SPME)对馒头挥发物质萃取效果的影响.结果显示:当样品用量为2 g(15 mL样品瓶),萃取温度为60℃,吸附时间为60 m in,解析温度和时间分别为250℃和4 m in时,提取到的挥发物质数量较多,主要挥发物质的萃取效果较好.馒头的挥发物质主要有醇类64.88%、羰基化合物4.29%、苯类3.81%、酯类2.75%、酰基化合物18.11%、杂环类6.14%.     

室内空气中酞酸酯类物质分析的研究

以固相微萃取（SPME）方法为前处理和分离手段采集室内空气中的酞酸酯类物质,进而在GC／MS上对其进行分析测定。通过对SPME中使用的极性与非极性纤维萃取头的萃取效果进行对比．确立了该类室内空气中酞酸酯类物质的分离和分析方法．并且比较了不同环境中室内各种邻苯二甲酸酯类的相对浓度大小。实验发现．与用传统的有机溶剂吸收空气中的化合物的方法相比．该方法可以检测出低浓度邻苯二甲酸二（2-乙基己基）酯（DEHP）．并且简化了实验过程．减少了干扰及有机溶液的使用量．并可以测定出浓度较低的酞酸酯类物质。     

Simulation of retronasal aroma of white and red wine in a model mouth system. Investigating the influence of saliva on volatile compound concentrations

The influence of saliva on aroma release from white and red wines was studied in a model mouth system. Aroma compounds were analysed in the dynamic headspace of wines by solid phase micro extraction/gas chromatography with flame ionization detection. Volatile compounds were identified by solid phase micro extraction/gas chromatography-mass spectrometry, resulting in a total of 43 compounds in white wine and 41 in red wine. The results showed a greater influence of saliva on aroma release in white wine than red wine. In white wine treated with human saliva, esters and fusel alcohols, responsible for fruity and fusel oil odours, were reduced of 32–80%; by contrast, the concentration of 2-phenylethanol and furfural, responsible for rose and toasted almond notes, increased by 27% and by 155%, respectively. In red wine, treated with human saliva, only a few esters decrease, with a reduction of 22–51% due to protein-binding ability of polyphenols that are able to inhibit the activity of the saliva. C-13 norisoprenoids, vitispirane (eucalyptol) and TDN (kerosene), decreased both in white and red wine, showing a comparable variation while, for β-damascenone, the variation was insignificant.     

Changes in Volatile Compounds of Black Cumin Oil and Hazelnut Oil by Microwave Heating Process

Black cumin and hazelnut oils were subjected to a heating process in a microwave oven for a duration of 2, 4, 6 and 8 min at a constant frequency of 2450 MHz and a power of 0.45 kW. The ultraviolet absorption and volatile products of the oils were investigated in detail during the processes. The experimental evidences obtained show that K₂₃₂ and K₂₇₀ parameters reach values of 4.69 and 1.30 for black cumin oil, 3.22 and 1.75 for hazelnut oil, respectively with the increment of heating time. The headspace SPME method was used to analyze volatile compounds extracted from black cumin and hazelnut oils being exposed to the microwave heating process. The SPME–GC/MS method allowed the detection of 17 identified volatile compounds (hexanal, α‐thujene, α‐pinene, sabinene, β‐pinene, 2‐heptenal, α‐terpinene, limonene, p‐cymene, γ‐terpinene, E‐2‐octenal, nonanal, 4‐terpineol, thymoquinone, E,E‐2,4‐decadienal, α‐longipinene and isolongifolene) in black cumin oils. Of the products, hexanal, 2‐heptenal, E‐2‐octenal, nonanal and E,E‐2,4‐decadienal were determined to be the predominant volatile oxidation products. In fact, the hexanal was found as a major volatile oxidation compound and reached a local maximum point of 7.41 × 10⁶ AU at the end of heating. On the other hand, only 8 volatile oxidation products (hexanal, heptanal, 2‐heptenal, nonanal, E‐2‐decenal, E,Z‐2,4‐decadienal, E,E‐2,4‐decadienal and E‐2‐tridecenal) were identified in hazelnut oils as a consequence of the heating process. Based on the experimental evidence observed, it is reasonable to conclude that the nonanal content dramatically increased at the end of heating and reached a value of 9.22 × 10⁶ AU.     

Solid-Phase Microextraction (SPME) of Pyrazines in Model Reaction Systems

Headspace solid-phase microextraction (HS-SPME) combined with gas chromatography (GC) was used for isolating and analysing pyrazines formed in a model system. This system consisted of an aqueous mixture of glucose, glycine and sodium hydroxide. Pyrazine formation was accelerated by heating in a microwave oven. Results were compared with our earlier ones using conventional techniques for isolation of pyrazines. HS-SPME-GC showed several advantages over traditional methods. The method is rapid, sensitive, easy to use and reproducible. Headspace and liquid of the model reaction were extracted and the results obtained using headspace sampling showed good agreement with the methylene chloride extraction method. In all cases, coefficients of variation of 5% or lower were obtained when the SPME extraction time was consistent.     

Investigating the Potential Use of Chemical Biopsy Devices to Characterize Brain Tumor Lipidomes

The development of a fast and accurate intraoperative method that enables the differentiation and stratification of cancerous lesions is still a challenging problem in laboratory medicine. Therefore, it is important to find and optimize a simple and effective analytical method of enabling the selection of distinctive metabolites. This study aims to assess the usefulness of solid-phase microextraction (SPME) probes as a sampling method for the lipidomic analysis of brain tumors. To this end, SPME was applied to sample brain tumors immediately after excision, followed by lipidomic analysis via liquid chromatography-high resolution mass spectrometry (LC-HRMS). The results showed that long fibers were a good option for extracting analytes from an entire lesion to obtain an average lipidomic profile. Moreover, significant differences between tumors of different histological origin were observed. In-depth investigation of the glioma samples revealed that malignancy grade and isocitrate dehydrogenase (IDH) mutation status impact the lipidomic composition of the tumor, whereas 1p/19q co-deletion did not appear to alter the lipid profile. This first on-site lipidomic analysis of intact tumors proved that chemical biopsy with SPME is a promising tool for the simple and fast extraction of lipid markers in neurooncology.     

Effect of sourdough fermentation on stabilisation,and chemical and nutritional characteristics of wheat germ

Lactic acid bacteria strains were identified from wheat germ by 16S rRNA partial sequencing, subjected to RAPD-PCR typing and screened. Lactobacillus plantarum LB1 and Lactobacillus rossiae LB5 were used as starters to produce sourdough fermented wheat germ (SFWG). The chemical and nutritional characteristics of SFWG were compared to those of the raw wheat germ (RWG). Lipase activity in SFWG was ca. 2.6-fold lower than that found in RWG. As shown by SPME/GC/MS analysis, most of the volatile compounds derived from lipid oxidation during storage (40 days) were at markedly lower levels in SFWG compared to RWG. Fermentation of wheat germ increased of ca. 50% the concentration of free amino acids. Glu markedly decreased in SFWG, due to its conversion in GABA. The concentration of the anti-nutritional factor raffinose also decreased in SFWG. The in vitro protein digestibility, the concentration of total phenols, phytase and antioxidant activities were increased by fermentation.     

Profiling of volatile compounds of Phyllostachys pubescens shoots in Taiwan

This study examined the influence of heating temperature and duration on volatile aromatic components of spring and winter Phyllostachys pubescens shoots using SPME. Results from GC–MS analyses revealed that the main constituents in both bamboo shoots at ambient temperature include methoxy-phenyl oxime, followed by n-hexanol and 3Z-hexenal, which gives a fresh green aroma. Comparing the different compounds, between spring and winter shoots, revealed that spring bamboo shoots at ambient temperature comprise 12.30% methyl salicylate, which provides protection against insect attack, and 9.71% epi-cedrol; while winter bamboo shoots comprise 17.00% 1-octen-3-ol, which produces a distinct mushroom aroma. After heating at 100 °C for 60 min, a marked increase in relative content of benzyl salicylate (43.30%) and a significant decrease in methyl salicylate content in spring bamboo shoots were observed; while the major compound in winter bamboo shoots was n-heneicosane (78.09%) and the content of specific 1-octen-3-ol significantly decreased.