Direct Determination of Polychlorinated-Biphenyls in Automotive Shredder Residues by Gas Chromatography-Mass Spectrometry

An easy and rapid method is proposed for the determination of PCBs in automotive shredder residues, using gas chromatography combined with low resolution mass spectrometry (GC-MS). It is based on direct n-hexane solid-liquid extraction, subtracting background of the lineal aliphatic hydrocarbon interferences and integration of chromatographic peaks containing selected ion PCBs masses (256, 292 and 326 m/z), which are common in all PCBs formulations. Recoveries were in the 80% - 120% range;PCBs were detected and quantified in shredder samples from an automotive shredder industry, thus indicating the validity of the method.

蒙山名茶蒙顶甘露和蒙山毛峰特征香气成分的GC-MS测定与分析

采用同时蒸馏萃取法和气相色谱质谱（gas chromatography-mass spectrometry ， GC-MS）分析方法系统分析了蒙山茶原产地保护区域内蒙泉、后盐、陇西3个产地及保护区外合江产地蒙顶甘露和蒙山毛峰香气成分的特征与差异.结果表明，在鉴定的63种香气成分中，醇类和醛类占一半以上（59.16％～71.42％）.在蒙顶甘露和蒙山毛峰的香气组分中均以植醇、香叶醇、L-芳樟醇、壬醛和正庚醛这5个成分所占比例较高；保护区内蒙顶甘露和蒙山毛峰最重要的香气特征是植醇和壬醛含量显著高于保护区外，其总量分别占保护区中心内甘露的29.95％和毛峰的40％、保护区外甘露的0％和毛峰的11.27％，同时也是区别于其他名优绿茶的最主要的香气成分.由保护区中心向外延伸，蒙顶甘露和蒙山毛峰的香型有相似的变化规律：由保护区中心的板栗香型经中间的铃兰类鲜爽花香型逐渐过渡至边沿的蜜糖香、花香型.总体上，原产地保护区域内蒙顶甘露和蒙山毛峰的香气品质优于其他非原产地保护区域的蒙顶甘露和蒙山毛峰.

广西八角挥发油的提取研究与GC-MS分析

In this paper,the Illilium verum Hook.f.grow at mountain of Dayao of Jinxiu in Guangxi,Volatile oil was extracted by soxhet method and steam distillation.All the volatile oil was analyzed by GC-MS,the result show the ingredients and rate of product were change greatly,The major chemical constituents were trans-anethole,estragole and anisaldehyde etc.

藏药甘肃蚤缀脂溶性成分的GC-MS分析

研究藏药甘肃蚤缀的脂溶性成分,进一步揭示该药材的化学成分,为这一传统藏药资源的开发利用提供实验依据。采用95%乙醇回流提取甘肃蚤缀全草,滤液浓缩后用石油醚萃取,得到脂溶性部位,通过气相色谱-质谱联用技术分析其化学成分,结合计算机检索技术及美国国家标准技术研究所(NIST)化合物谱库检索进行鉴定,采用面积归一化法确定其相对含量。从甘肃蚤缀石油醚部位共分离鉴定出25个化合物,相对含量占总含量的91.31%,包括脂肪类、甾体、三萜及芳香化合物等。

基于GC-FID、HS-SPME-GC-MS与电子鼻技术评价不同水果发酵酒的香气特征

采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry,HS-SPME-GC-MS)和电子鼻技术分析6种果酒中的挥发性成分,评价果酒风味轮廓特征的差异性。结果表明,GC-FID定量测定樱桃李酒,其中异戊醇、活性戊醇、β-苯乙醇含量最高,乙酸乙酯含量最低;木瓜酒中正丙醇、2,3-丁二醇、癸酸乙酯、乙酸含量最高; 3-羟基-2-丁酮含量在樱桃李酒中最高,山楂酒、甜橙酒中最少。HP-SPME-GC-MS鉴定果酒中挥发性物质94种,其中醇类23种,酯类43种,醛酮类10种,酸类8种,酚类2种,苯环类5种,烷烃类3种。山楂酒、菠萝酒、木瓜酒、甜橙酒、无花果酒和樱桃李酒中香气物质数量分别为34、44、45、45、33、47种。其中山楂酒、木瓜酒和无花果酒中未检出酚类、烷烃类物质。电子鼻对不同果酒香气的区分效果无重叠,W5S传感器区分果酒香气能力最强。比较而言,菠萝酒和樱桃李酒的口感更圆润,香气更愉悦,感官得分最高。

福建姜黄挥发油化学成分的HS-SPME-GC-MS分析

采用水蒸气蒸馏法提取福建姜黄挥发油,应用顶空固相微萃取进样结合气相色谱-串联质谱联用技术(HS-SPME-GC-MS)分析姜黄挥发油的化学成分。结果表明:姜黄挥发油含有量为7.2%(mL/g),从姜黄挥发油中共分出62个色谱峰,初步鉴定出了其中的51种化学成分,占总挥发油总量的98.41%。在鉴定的化合物中,主要为单萜类化合物和倍半萜类化合物,其中新发现一种主要成分为β-柏木烯,相对含量占比高达26.58%,这可作为福建姜黄挥发油的特征成分和主要品质指标。本研究结果将为福建姜黄植物药材的品质评价提供科学依据。

GC-MS法测定黄酒和食用酒精中的氨基甲酸乙酯

建立应用气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)快速测定黄酒和食用酒精中氨基甲酸乙酯(ethylcarbamate,EC)的分析方法。以黄酒和食用酒精为研究对象,样品经过碱性硅藻土固相萃取柱净化、浓缩后,用GC-MS进行测定,同位素内标法定量。氨基甲酸乙酯在10~600μg/L线性关系良好,相关系数r^2=0.999 3。加标水平为5、100、250μg/kg 3个浓度条件下,在黄酒中的加标回收率为81.2%~89.5%,每个加标水平测定6次的相对标准偏差(RSD)为3.7%~5.0%;在食用酒精中的加标回收率为91.2%~99.4%,每个加标水平测定6次的RSD为3.1%~4.1%。方法的检出限为1.0μg/kg,方法的定量限为3.0μg/kg。该方法定量准确、操作简便、灵敏度高,适用于黄酒和食用酒精中氨基甲酸乙酯的测定。

Determination of Aromatic Components of Rosa davurica Pall. by Headspace Solid Phase Microextraction Combined with GC-MS

[Objectives] To determine the aromatic components of Rosa davurica Pall. [Methods] 42 kinds of aromatic components were identified from the flowers of R. davurica by headspace solid phase microextraction( HS-SPME) combined with gas chromatography-mass spectrometry( GC-MS). The main compounds were alcohols( 54. 88%) and aldehydes( 19. 55%). [Results] The top five components with the highest relative content were phenylethyl alcohol( 12. 69%),geraniol( 9. 85%),citronellol( 8. 80%),nerol( 7. 84%) and 2-n-pentylfuran( 7. 45%). [Conclusions] Headspace solid phase microextraction( HS-SPME) combined with gas chromatography-mass spectrometry( GC-MS) can provide basis for further development and utilization of R. davurica.

Studies on the Components of Essential Oil of <i>Zanthoxylum Armatum</i>by Gc-Ms

The essential oil of Zanthoxylum armatum was extracted through hydro distillation and analyzed by GC-MS. Hydrocarbon fraction (17.35%) of the oil was much lower and oxygenated compounds comprised fairly high portion of essential oil (39.21%). Percentages of monoterpenes and sesquiterpenes found were 47.33% and 10.83% respectively. Oxygenated monoterpenes comprised major profile of chromatogram of essential oil of Zanthoxylum armatum i.e. 37.23% where as monoterpene hydrocarbons were 10.09%. Alcoholic percentage was much higher i.e. 26.76% and 15-hexadecanoloide (6.58%) the only cyclic ester was found in relatively high percentage.

Study on the Difference between Volatile Constituents of the Different Parts from <i>Elsholtzia ciliata</i>by SHS-GC-MS

In this study, the comparison of Elsholtzia ciliata volatile compounds from the stem (with leaf) and flower was acquired. The volatile compounds of these two parts from Elsholtzia ciliata aerial parts were respectively analyzed by a rapid and convenient static headspace injection technique coupled with gas chromatography-mass spectrometry and the relative contents of each constituent between the two different parts were determined by peak area normalization. 61 compounds were identified in the stem (with leaf) and flower, among which 39 components simultaneously exist. 47 and 53 compounds were separated and identified in the volatile compounds from the different parts of Elsholtzia ciliata, respectively. There were differences among some volatile constituents of the two parts, but the main constituents were all Elsholtzia ketone, caryophyllene, 3-octanol and Dehydroelsholtzia ketone. The most abundant components in the stem (with leaf) included Elsholtzia ketone (84.20%), caryophyllene (4.3%) and 3-octanol (3.11%), while Elsholtzia ketone (88.03%), caryophyllene (3.33%) and 3-octanol (1.53%) were the main components in the flower. 8 single constituents were identified in the stem (with leaf) volatiles including 3-heptanone and linalool, while 14 constituents only including 2-methylbutanoic acid and Perillene have been found in the flower volatiles. Elsholtzia ketone was the main compound, and its concentration was significantly higher than other substances (>80% of the total oils in Elsholtzia ciliata). The study provided an important scientific base for the further utilization of Elsholtzia ciliata resources and may be helpful for systematically understanding the constituents of volatile compounds of Elsholtzia ciliata.

GC-MS Analysis and Antibacterial Activity Study of Volatile Oil from 11 Kinds of Aurantii Fructus Immaturus Processed Products

[Objectives]To study the volatile components and antibacterial effects of 11 kinds of Aurantii Fructus Immaturus processed products.[Methods]11 kinds of Aurantii Fructus Immaturus processed products were obtained according to the traditional processing method,the volatile oil was extracted by steam distillation,and the composition of volatile oil in the 11 kinds of processed products was analyzed by gas chromatography-mass spectrometry(GC-MS).the relative percentage content of each component in these 11 kinds of processed products was determined using the peak area normalization.The drug sensitivity activity of the volatile oil of these 11 kinds of processed products was tested using the K-B paper diffusion method and the minimum inhibition volume fraction of volatile oil of these 11 kinds of processed products was tested using the microdilution method.[Results]The highest yield of volatile oil of 11 kinds of these processed products was baking(5.193%),and the lowest was stir-bake to scorch(1.998%).A total of 36 chemical components were identified from the volatile oils of these 11 kinds of processed products.The components with the most volatile oil were stir-bake to scorch(24 kinds),and the components with the least volatile oil were the method of processing with rice-washed water(15 kinds).They contain 8 kinds of common chemical components,such as limonene,linalool,myrcene,α-pinene.The highest content of limonene came from processing with honey(60.93%),the lowest came from processing with rice-washed water(55.25%);the highest content of linalool came from processing with rice-washed water(7.139%),the lowest came from processing with honey(5.436%);the highest content of myrcene came from processing with honey(1.899%),the lowest came from stir-bake to scorch(1.632%);the highest content ofα-pinene came from raw Aurantii Fructus Immaturus(2.355%),and the lowest came from stir-bake to scorch(1.618%).The volatile oil of these 11 kinds of Aurantii Fructus Immaturus processed products has good antibacterial effect on Escherichia coli and Staphylococcus aureus.[Conclusions]The oil yields of volatile oils of 11 kinds of Aurantii Fructus Immaturus processed products are different,the content of limonene is significantly different,and the changes of other chemical components and their contents are not significantly different.The volatile oil of 11 kinds of Aurantii Fructus Immaturus processed products has certain antibacterial effect.

Analysis of the Volatile Components of Polygonum chinense L.Extracted with Different Solvents by GC-MS

[Objectives]This study was conducted to investigate the volatile components of Polygonum chinense L.[Methods]The volatile components of the methanol extract,ethyl acetate extract,chloroform extract and petroleum ether extract of P.chinense were analyzed and determined by gas chromatography.[Results]The volatile components of the methanol extract from P.chinense were the most,and phenolic acids and ketones accounted for a relatively high proportion,among which pyrogallic acid had the highest content.The ethyl acetate extract contained the second most volatile components,mostly acids and esters,of whichβ-sitosterol had the highest content;the chloroform and petroleum ether extracts had relatively few types of volatile components,most of which were alkanes,and the content ofγ-sitosterol shared by the two was the highest.The common substances of the four extracts were palmitic acid and phytol.[Conclusions]This study provides a theoretical basis for the quality evaluation of P.chinense and a scientific basis for its resource development.

Rapid on-site identification of hazardous organic compounds at fire scenes using person-portable gas chromatography-mass spectrometry(GC-MS)—part 1:air sampling and analysis

Recent advancements in person-portable instrumentation have resulted in the potential to provide contemporaneous results through rapid in-field analyses.These technologies can be utilised in emergency response scenarios to aid first responders in appropriate site risk assessment and management.Large metropolitan fires can pose great risk to human and environmental health due to the rapid release of hazardous compounds into the atmosphere.Understanding the release of these hazardous organics is critical in understanding their associated risks.Person-portable gas chromatography-mass spectrometry(GC-MS)was evaluated for its potential to provide rapid on-site analysis for real-time monitoring of hazardous organic compounds at fire scenes.Air sampling and analysis methods were developed for scenes of this nature.Controlled field testing demonstrated that the portable GC-MS was able to provide preliminary analytical results on the volatile organic compounds present in air samples collected from both active and extinguished fires.In-field results were confirmed using conventional laboratory-based air sampling and analysis procedures.The deployment of portable instrumentation could provide first responders with a rapid on-site assessment tool for the appropriate management of scenes,thereby ensuring environmental and human health is proactively protected and scientifically informed decisions are made for the provision of timely advice to stakeholders.

Exploring Chemovar-Specific Cannabis Extracts Quantification and Evaluation of Cytotoxic Compounds for Targeting Glioblastoma Multiforme

Glioblastoma Multiforme (GBM) represents one of the most aggressive and metastatic brain tumors, with a dismal success rate of less than three percent after five years, particularly in tumors with active immune checkpoints. This necessitates the development of targeted endogenous agents for precise GBM treatment. Previous experiments utilizing Chemovar Specific Cannabis Extractions (CSCEs), fractionated with polar solvents and quantified using Liquid and Gas Column Chromatography combined with Mass Spectrometry (LC/GCMS), have shown reduced viability and motility in human GBM cell lines. However, the complexity of the botanical substance has hindered the personalization of standard cannabis medicines for GBM due to unknown synergistic effects of multiple compounds. To address this limitation, our study focuses on exposing AM251 cells to chemovar fractions extracted using a non-polar solvent, thereby isolating a broader spectrum of constituents. By employing LC/GCMS in conjunction with Nuclear Magnetic Resonance (NMR), we have identified and quantified nine* compounds present in the non-polar CSCE that exhibit significant efficacy (0.1 μM) in inducing cytotoxicity* in GBM tumor cells. Conversely, the polar fraction in our experiment did not demonstrate efficacy against UM251 cells. The quantification of individual compounds within a cannabis extraction that selectively induces cell death in brain tumors holds promise for guiding future research and facilitating the development of a standardized CSCE for GBM therapy.

从姜黄及姜黄浸膏中提取的挥发油化学成分研究

The volatile oil was extracted from Curcuma longa and Turmeric oleoresin by Soxhelt method with petroleum ether.All the volatile oil was analyzed of chemical component by the method of GC-MS,the relative contents of these compounds were calculated using square peaks to normalization.On the volatile oil of Curcuma longa 35 peaks were separated and 21 compounds were identified,which accounted for 89.10%,the main chemical constituents was (-)-Zingiberene(22.12%),β-Sesquiphellandrene(15.24%),α-Turmerone (11.30%),β-Turmerone (8.87%),Ar-turmerone(8.20%),but on the volatile oil of Turmeric oleoresin 32 peaks were separated,of which 21 compounds were identified,which accounted for 90.12% the main chemical constituents was (-)-Zingiberene(23.92%),β-Sesquiphellandrene(15.73%),Ar-turmerone(12.89%),β-Turmerone(10.85%).

气相色谱-质谱法对乳化炸药及其残留物中特征组分的分析

The emulsible explosives and its post-blast residues were analyzed by gas chromatography-mass spectrometry(GC-MS).A sensitive analysis method has been established.

松木屑催化热解及热解油分析

以松木屑为原料,选取无水Na2CO3、无水Al2O3、凹凸棒土、ZSM-5共4类催化剂,利用管式炉实验及色质联用(GC-MS)分析仪进行热解特性研究,探索了热解产物产率和组分特性的变化规律.实验结果表明,松木屑在热解温度为550,℃时,产油率达到最大值51.47%(质量分数);无催化剂条件下松木屑热解油主要成分为酸类化合物,加催化剂条件下松木屑热解油主要成分为酸类和酮类化合物,催化剂的加入主要影响了呋喃类、醇类、糖类和含氮类化合物的质量分数.ZSM-5催化剂的催化性能最佳,其能够提高热解油产率,其对应的热解油中酯类、呋喃类和芳香族类等能够提高热解油品质的化合物质量分数均较高,而糖类、含氮类等化合物质量分数较低,能够提高热解油的稳定性.

柠檬烯纳米脂质体的制备及其性质测定

以柠檬烯为原料,利用乙醇注入法制备柠檬烯纳米脂质体。在单因素试验基础上,以胆固醇添加量、柠檬烯添加量、磷酸盐缓冲溶液(phosphate buffer solution,PBS)的温度为影响因素,以包封率为响应值,根据BoxBehnken试验设计原理,采用3因素3水平的响应面分析法优化柠檬烯脂质体的制备工艺,得到柠檬烯脂质体的最佳制备工艺条件为:胆固醇的添加量为8.8 mg、柠檬烯添加量为12.7 mg、PBS温度为51℃,在此条件下柠檬烯纳米脂质体的包封率为(67.44±0.58)%,与模型预测值相对误差为0.4%,重现性良好,平均粒径为(165.4±2.08)nm,PDI为(0.185±0.011),Zeta电位值为(-16.23±0.569)m V。

不同等级金华火腿挥发性风味物质分析

采用热脱附-气相色谱-质谱联用(thermal desorption-gas chromatograph-mass spectrometer,TD-GC-MS)检测不同等级、不同部位金华火腿挥发性风味物质。结果表明:不同等级的金华火腿挥发性风味物质具有很大的差异,相同等级金华火腿不同部位之间差别也很大。特级火腿第一签中甲苯、苯甲醛和壬醛的相对含量最高,分别达到11.74%、9.93%和8.64%;第二签中γ-丁内酯、壬醛和甲苯相对含量最高,分别达到10.49%、10.23%和8.76%;第三签中壬醛、异戊酸、2-戊基呋喃相对含量最高,分别达到14.12%、8.69%和8.01%。一级火腿第一签中2-戊基呋喃、己醛和壬醛的相对含量最高,分别达到17.85%、14.70%和12.07%;第二签中苯酚、四氢香叶醇和甲苯相对含量最高,分别达到44.81%、17.43%和4.04%;第三签中己醛、四氢香叶醇、α-蒎烯相对相对含量最高,分别达到25.75%、13.89和6.90%。二级火腿第一签中壬醛、己醛和反式-2-癸烯醛的相对含量最高,分别达到14.91%、12.71%和6.89%;第二签中己醛、2,3,5,6-四甲基吡嗪和正丁酸相对含量最高,分别达到23.74%、15.82%和6.58%;第三签中壬醛、己醛、δ-壬内酯相对含量最高,分别达到19.27%、15.28%和5.59%。

林芝松口蘑与红菇蜡伞子实体香气成分比较

研究采用顶空固相微萃取技术联合气质联用技术分别对松口蘑和红菇蜡伞子实体香气成分进行分析测定和比较分析,以期建立准确、快速、高效的鉴别方法。结果显示,松口蘑检测到74种香气成分,红菇蜡伞检测到72种香气成分,松口蘑相较红菇蜡伞检测到特有的香气成分14种,包括乙醛、庚醛等6种醛类,2(5H)-呋喃酮1种酮类,3-苯丙醇1种醇类,正己酸乙酯、丙位戊内酯2种酯类,萜品烯和异松油烯等4个烯烃类;红菇蜡伞相较松口蘑,检测到特有的香气成分16种,包括2-丁基-2-辛烯醛1种醛类,3-羟基-2-丁酮、甲基庚烯酮等4种酮类,丁醇等5种醇类,(1-羟基-2,4,4-三甲基戊-3-基) 2-甲基丙酸酯1种酯类,异丁酸、丁酸等3种羧酸类,邻甲酚1种酚类,乙二醇单丁醚1种醚类,N-甲基吡咯烷酮1种含氮化合物。经过主成分分析,得到红菇蜡伞中的主要特征性香气成分为:己醛、3-羟基-2-丁酮、3-辛烯酮、2-甲烯基丁内酯、异戊酸;松口蘑中为:异戊醛、庚醛、壬醛、2,5,2-三甲基吡嗪、2,6,2-三甲基吡嗪。同时对松口蘑与红菇蜡伞干品挥发性香气成分相对含量对比发现,松口蘑主要香气成分含量关系为醛类>烯烃类>醇类>酯类,红菇蜡伞主要香气成分含量关系为醛类>醇类>烯烃类>酯类。通过松口蘑与红菇蜡伞子实体干品香气成分的比较分析可为市售的2种产品的快速检验鉴别奠定理论基础。