猕猴桃果酒香气成分的气相色谱/质谱分析

采用溶液萃取法提取猕猴桃果酒中的香气成分，经气相色谱－质谱联机分析，分离出44个峰，鉴定出42种化合物，占总峰面积的94．51％。其中主要为3－甲基丁醇、2－甲基丙醇、苯乙醇、乙酸乙酯、四氢化2－甲基噻吩、辛酸、二氢化－2（3H）－呋喃酮、乙酸3－甲基丁酯、己酸、1H－吲哚－3－乙醇等。     

用台式色谱-质谱仪同时进行原油芳烃色谱和色谱-质谱分析

用ＨＰ６８９０ＧＣ／５９７３ＭＳＤ仪器,一次进样同时测定原油、烃源岩抽提物中芳烃馏分的芳烃色谱和色谱－质谱信息,效果良好,在有机地球化学研究工作中很有实用价值,方法具有高效、经济等优点。     

色谱／质谱联用技术分析测定贻贝中的多环芳烃

介绍了ＧＣ－ＭＳ联用技术－物质征离子选择法测定贻贝中多环芳烃的分析方法，并就定性定量离子的选择，以及方法的准确度和精密度进行了探讨。结果表明，本方法适用于海洋生物贻贝，牡蛎中ＰＡＨｓ的分析测定。     

气相色谱/质谱法测定熏肉中的多环芳烃

建立了熏肉中多环芳烃的气相色谱/质谱(GC/MS)测定方法。样品经正己烷-丙酮(体积比为1∶1)超声波提取、氧化铝柱净化后,用GC/MS分离测定。优化了25种多环芳烃(PAHs)化合物的分离测定条件。结果 25种PAHs回收率范围为48.5%-106.5%;日内(n=7)相对标准偏差为3.75%-7.95%。方法具有灵敏度高、准确度好、能同时分离测定20余种多环芳烃化合物的优点,适合于熏肉中多环芳烃化合物的分析测定。     

界面衍生化气相色谱法测定葡萄酒中总有机酸

利用离子交换树脂分离、富集葡萄酒中总有机酸并直接在树脂界面上乙酯化,结合气相色谱／质谱法,鉴定并分析了葡萄酒中２１种有机酸。     

焦炉烟气中全量多环芳烃分析方法

报道了利用处在制串联采样装置。优选出了比较理想的前处理方法，并用此方法对焦炉烟气中的全量多环芳烃进行了研究。滤膜颗粒物中的多环芳烃有６途中 ，聚氨酯泡沫吸附剂中有４９种。     

Comparative Evaluation of Red Wine from Various European Regions Using Mass Spectrometry Tools

The goal of this work was to assess differences in the composition of red wine produced in Poland, Hungary, Moldova, and Bulgaria, related to their geographical origin. Inductively coupled plasma–mass spectrometry results obtained for 23 elements were submitted to principal component analysis, indicating the association of Li, Co, Se, Cu, Sr with Moldovan products; Hungarian and Moldovan wines were characterized by V, As, Al, Fe variables, whereas Be was distinctive for Hungarian products. Polish wines were grouped with Cd and Pb and Bulgarian with Tl, Ba, Rb, and Mo; U and Mn were found as characteristic variables for wines from Bulgaria and Moldova. According with current legislation, the investigated wines were not contaminated with heavy metals and might be even considered a good source of essential elements (Cu, Mn, Fe, Zn, Cr, and Co). Gas chromatography–high-resolution time-of-flight mass spectrometry was used as a complementary analytical tool, targeting nonvolatile organic compounds amenable for silylation. Statistical data analysis revealed that geographical factors strongly affected the metabolic profiles. Specifically, 15 compounds presenting higher abundances in Bulgarian as compared to Polish wines were found, including monosaccharides, polyols, organic acids, sugar acids, and the amino acid proline. The highest fold change was obtained for ribose (37.9), followed by proline (12.2) and inositol (5.68), suggesting that these compounds might be especially useful for discrimination purposes. The obtained results encourage for further studies aimed at the discrimination of wine produced over the entire Central-East European region based on metal/metalloid profiling and on the evaluation of specific metabolites.     

Simultaneous determination of 20 components in red wine by LC‐MS: Application to variations of red wine components in decanting

The decanting of red wines has a long tradition in red wine service from the perspective of modifying the aroma or taste of a wine. A simple and sensitive liquid chromatography‐mass spectrometry method was developed for the simultaneous determination of 20 organic acids and polyphenols in decanting red wine. The separation was performed on a Diamonsil C₁₈ column (250 mm × 4.6 mm, 5 μm) using a mobile phase composed of methanol‐0.1% acetic acid under gradient elution. Analysis was performed in selected ion monitoring mode with negative electrospray ionization interface. All the linear regressions showed good linear relationships (r² > 0.9973) between the peak area and concentration of each marker. The assay was reproducible with overall intra and interday variation of less than 5.0%. The recoveries for the quantified compounds were observed over the range of 92.1–108.3% with RSD values less than 5.7%. The method developed was successfully applied to determine the variations of the 20 components in red wine after decanting in different conditions. Concentrations of most organic acids and polyphenols investigated in the red wine were decreased in decanting. In addition, increment of duration, temperature, and light intensity would intensify the changes.     

Flavor components in tobacco capsules identified through non-targeted quantitative analysis

Tobacco flavors increase the attractiveness of a tobacco brand and ultimately promote addiction. Information about what flavor and how much flavor is in flavor capsules can provide an effective way to regulate tobacco flavor. In this study, 128 flavor chemicals were identified and quantified by gas chromatography–mass spectrometry using libraries and authentic standards. Validation of the developed method was performed for interference, detection limits, calibration curves, accuracy, and precision. Menthol was the main ingredient in all capsules, and the carcinogenic pulegone was detected. Detected menthofuran, benzyl alcohol, geraniol, and eugenol cause toxic or severe irritation, and detected lactones can increase nicotine addiction by inhibiting nicotine metabolism in smokers. Margin of exposures for carcinogenic pulegone and non-carcinogenic menthol were well below safety thresholds, indicating a significant risk of inhalation exposure. It is desirable to prohibit the use of flavor capsules in consideration of human risk.     

A GC-MS Protocol for the Identification of Polycyclic Aromatic Alkaloids from Annonaceae

The Annonaceae are an old family of flowering plants belonging to the order Magnoliales, distributed mainly in tropical regions. Numerous Annonaceae species find ethnobotanical use for curing a broad range of diseases, among them cancer and infections by diverse pathogens. Hence, bioactive natural products from Annonaceae have received considerable interest in drug development. Beyond cytotoxic acetogenins, unique aporphine-derived polycyclic aromatic alkaloids are characteristic constituents of Annonaceae. Among them are unique tri- and tetracyclic aromatic alkaloids like azafluorenones, diazafluoranthenes, azaanthracenes, and azaoxoaporphines. The complex substitution pattern of these alkaloids represents a major challenge in structure elucidation of isolated natural products. Based on a broad spectrum of alkaloids available from our previous work, we present a GC-MS protocol for the identification of over 20 polycyclic aromatic alkaloids from Annonaceae. This collection of data will contribute to the future identification of the metabolite patterns of extracts from Annonaceae as an important source of novel bioactive secondary metabolites.     

Identification and quantification of diesel fuel components derived from off-shore drilling operation discharges

A GC/MS technique that provides quantitative and qualitative information on diesel fuel components in drilling muds is described. Several low molecular mass aromatic components of diesel fuel are identified as indicators of diesel fuel. The presence and relative concentration of these indicators is used to identify diesel fuel contamination. This information can be used to approximate the amount of diesel fuel contamination in off-shore drilling discharges.     

薄荷卷烟中香味成分的全二维气相色谱/飞行时间质谱分析

采用全二维气相色谱/飞行时间质谱法(GC×GC/TOFMS),以较长的非极性柱DB-5MS(30m×0.25mm×0.25μm)作为第一维柱,较短的中等极性柱DB-17MS(2m×0.1mm×0.1μm)作为第二维柱,利用固相微萃取法作为香味成分的萃取方法,对薄荷型ESSE卷烟的核心香味成分进行了定性分析,TOFMS谱图库检索结合全二维特有的包含结构信息的二维谱图,通过族分离和结构谱图鉴定,共鉴定了187种挥发性成分,其中对香气有贡献的成分118种.     

食品中胆固醇色谱／质谱／质谱的测定

确立了用色谱／质谱／质谱测定食品中胆固醇的一种新方法，试样经乙酸乙酯提取后，ＧＣ／ＭＳ／ＭＳ测定分析，以胆固醇分子离子为母离了，以其子离子为定量分析的碎片离子。线性好，回收率高，方法可靠。     

Chemometric approach to the optimisation of LC-FL and GC-MS methods for the determination of nitrite and nitrate in some biological,food and environmental samples

Gas chromatography–mass spectrometry (GC-MS) method and a liquid chromatography–fluorescence (LC-FL) detection method using experimental design and optimisation approach were improved for the quantitative determination of nitrite and nitrate in biological, food and environmental samples. The obtained recoveries of nitrite and nitrate ions from samples based on both GC-MS and LC-FL results ranged from 98.5% to 98.9% for nitrite and 97.9% to 98.4% for nitrate. The precision of these methods, as indicated by the relative standard deviations (RSDs), was within the range from 2.4% to 3.6% for nitrite and 2.5% to 3.8% for nitrate, respectively. The limits of detection of nitrite and nitrate ions from samples based on GC-MS and LC-FL results ranged from 0.01 to 0.14 ng L^?1 for nitrite and 0.02 to 0.71 ng L^?1 for nitrate, respectively. The optimised isolation procedure by central composite design was successfully applied to real samples. The results revealed that the proposed procedure combined with GC-MS and LC-FL techniques is more sensitive, reliable and selective compared to the other methods available for the precise determination of trace levels of nitrite and nitrate in biological, food and environmental samples.     

Characterization of Catalysts for Glycerol Ester Production with Various Acetylating Agents

The use of raw materials from renewable sources by industries is essential to the sustainable development of modern society. The biodiesel produced by the transesterification of vegetable oils is a less polluting diesel fuel, but large amounts of glycerol (10% of total weight of product) are generated during the production process. The scientific community and industries of the sector know that, in the future, the amount of glycerol generated can cause a serious ecologic problem. Thus, it is essential to find alternatives for the consumption of this co-product, in its crude form and/or as high value-added derivatives. This work studied obtaining triacetate from the glycerol esterification reaction that was determined by electrospray ionization–mass spectrometry and gas chromatography–mass spectrometry. The reactions were carried out with sulfuric acid, phosphotungstic acid and in the absence of catalyst, using different acetylating agents (acetic acid and acetic anhydride). The phosphotungstic acid showed satisfactory performance in the catalytic esterification of glycerol when acetic acid and acid anhydride were used. The use of acetic anhydride as the acetylating agent favors the esterification reaction, decreasing the reaction time required for obtaining glycerol triacetate.     

Characterization of odorous contaminants in post‐consumer plastic packaging waste using multidimensional gas chromatographic separation coupled with olfactometric resolution

The increasing world population with their growing consumption of goods escalates the issue of sustainability concepts with increasing demands in recycling technologies. Recovery of post‐consumer packaging waste is a major topic in this respect. However, contamination with odorous constituents currently curtails the production of recycling products that meet the high expectations of both consumers and industry. To guarantee odor‐free recyclates, the main prerequisite is to characterize the molecular composition of the causative odorants in post‐consumer plastic packaging waste. However, targeted characterization of odorous trace contaminants among an abundance of volatiles is a major challenge and requires specialized and high‐resolution analytical approaches. For this aim, post‐consumer packaging waste was characterized by sensory analysis and two‐dimensional high resolution gas chromatography coupled with mass spectrometry and olfactometry. The 33 identified odorants represent various structural classes as well as a great diversity of smell impressions with some of the compounds being identified in plastics for the first time. Substances unraveled within this study provide insights into sources of odorous contamination that will require specific attention in the future in terms of screening and prevention in recycling products.     

气相色谱-质谱联用法分析北大仓白酒香气成分

利用溶剂萃取法进行分离和富集,采用气相色谱-质谱联用技术对北大仓白酒香气成分进行分析。从北大仓白酒的二氯甲烷萃取物中分离并鉴定了30种物质,其中酯类22种,占所有香气物质的94.847%;酸类2种,占4.659%;烷烃类2种,占0.228%;醇类2种,占0.185%;酮类1种,占0.060%;酸酐类1种,占0.021%。所含主要化合物为己酸乙酯、2-羟基丙酸乙酯和己酸,合计占总香气成分的96.396%,构成了北大仓白酒香气成分的骨架。     

超高效液相色谱-电喷雾串联质谱法直接测定黄酒和葡萄酒中氨基甲酸乙酯

建立了超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)直接测定黄酒和葡萄酒中氨基甲酸乙酯含量的方法。黄酒和葡萄酒样品经蒸馏水简单稀释后,过0.22 μm微孔滤膜,直接进行UPLC-MS/MS分析检测。以Waters Acquity UPLCTMBEH C18色谱柱为分析柱,乙腈和0.1%(v/v)乙酸水溶液为流动相,采用电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,以氨基甲酸丁酯(BC)作为内标进行定量。结果表明: 方法在2～500 μg/L的范围内线性关系良好(相关系数大于0.995),其对黄酒和葡萄酒的检出限为1.7 μg/L,定量限为5.0 μg/L,可达到黄酒和葡萄酒中氨基甲酸乙酯的检测要求。当添加水平为10、20和100 μg/L时,黄酒和葡萄酒中待测组分的回收率为90%～102%,日内精密度(n=6)为0.8%～4.5%,日间精密度(n=6)为1.4%～5.6%。该方法样品处理简单,前处理过程不使用有机溶剂,测定快速、准确,灵敏度高,非常适合黄酒和葡萄酒中氨基甲酸乙酯的快速检测和定量分析。     

茶叶香味扫描和挥发性化学成分分析

为区分不同茶叶的香味，利用电子扫描仪对铁观音、兰贵人、玉针、碧螺春和云雾茶等5种茶叶进行了香味扫描，确定了电子鼻在茶叶香味辨别中的作用。采用固相微萃取．气相色谱／质谱联用法对这5种茶叶样品中的挥发性化学成分进行了定性和定量分析，分别鉴定出40、40、35、16和13种化合物。在鉴定出的化学成分中，乙酸、大茴香醚、十六烷、咖啡因、十六酸和双酚A是5种茶叶样品中所共有的化学成分，每种茶叶样品中又都含有一些特有的化学成分。最后对香味扫描结果和挥发性化学成分分析结果进行了分析，研究了挥发性化学成分组成和含量上的差别，对茶叶样品数据点在香味分析三维图中位置的影响。     

Impact of Milling on Rice Constituents (Oryza Sativa L.): A Metabolomic Approach

Milling is an influential factor that affects the nutritional components in rice. However, the alteration of rice constituents by milling has not been thoroughly examined. In this study, rice with various degrees of milling was analyzed by gas chromatography–mass spectrometry and high-performance liquid chromatography–mass spectrometry. Principal component analysis and partial least square-discriminant analysis were performed to characterize the nutritional components that have significant changes during milling. The concentrations of sugars and sugar alcohols decreased while the phospholipids increased in accordance with the milling degree. These results provide a contrast to the common idea that brown rice is nutritionally superior to white rice. In conclusion, the knowledge of nutritional alterations related to milling may benefit rice production and consumption.