Determination of Aroma Composition of Santalum album Linn by Solid-phase Microextraction-Gas Chromatography-Mass Spectrometry

[Objectives]This study aimed to determine the volatile components in Santalum album Linn and gradually clarify the aroma composition of S.album Linn.[Methods]Solid-phase microextraction method was used to obtain the volatile components of S.album Linn.The aroma components were analyzed by gas chromatography-mass spectrometry and their relative contents were calculated using the area normalization method.[Results]In a dry state at room temperature,39 chemical components were identified from S.album Linn,mainly olefins(91.15%),alkanes(3.00%),alcohols(2.56%),esters(2.19%),ketones(0.55%),aldehydes(0.41%)and heterocyclics(0.14%).[Conclusions]This method has the advantages of low sample consumption,easy operation,rapid identification of aroma components and high sensitivity,and can effectively separate and determine volatile components in S.album Linn,realizing the rapid identification of different S.album Linn varieties and providing technical support for further research on Chinese medicinal materials.

Multiresidue Method for Determination of 67 Pesticides in Water Samples Using Solid-Phase Extraction with Centrifugation and Gas Chromatography-Mass Spectrometry

A new multi-residue method based on solid-phase extraction (SPE) with centrifugation was developed for determination and quantitation of 67 pesticides in water samples. Two SPE cartridges were tested: Chromabond C18 and Oasis HLB. Parameters that influence the extraction efficiency such as the eluent volume, the sample loading volume, the addition of organic solvent to water sample, sorbent drying and elute concentration were optimized. The innovation of this work was the examination of the use of a centrifugation technique in both the drying and elution steps. When combined with centrifugation, the volume of the elution solvent was reduced to 2 mL and the time for sorbent drying decreased also to 10 min under vacuum. Under the optimized conditions, this method showed good recoveries higher than 65% - 68% for the 67 analyzed pesticides using the C18 and HLB cartridges with relative standard deviations lower than 9.7% - 12.3%. Limits of quantification were between 2 and 20 ng.L–1. The simplicity of the described method, use of less of organic solvent, short procedure time, and good recoveries demonstrate the advantages of this environmentally friendly approach for routine analysis of numerous samples.

Comparison of simultaneous distillation extraction and solid-phase micro-extraction for determination of volatile constituents in tobacco flavor

The volatile and semi-volatile components in tobacco flavor additives were extracted by both simultaneous distillation extraction and solid-phase micro-extraction. Extraction conditions for solid-phase micro-extraction were optimized with information theory. Then, detection were accomplished by gas chromatography-mass spectrometry. Characteristic of each method was compared. Qualitative analysis and quantitative analysis of 6# tobacco flavor sample were accomplished through both simultaneous distillation extraction and solid-phase micro-extraction. The experimental results show that solid-phase micro-extraction method is the first choice for qualitative analysis and simultaneous distillation extraction is another good selection for quantitative analysis. By means of simultaneous distillation extraction, 20 components are identified, accounting for 92.77% of the total peak areas. Through solid-phase micro-extraction, there are 17 components identified accounting for 91.49% of the total peak areas. The main aromatic components in 6# tobacco flavor sample are propanoic acid, 2-hydroxy-, ethyl ester, menthol and menthyl acetate. The presented method has been successfully used for quality control of tobacco flavor.

Preparation of polypyrrole/nanosilica composite for solid-phase microextraction of bisphenol and phthalates migrated from containers to eye drops and injection solutions

This paper describes the electrodeposition of polyphosphate-doped polypyrrole/nanosilica nano-composite coating on steel wire for direct solid-phase microextraction of bisphenol A and five phthalates. We optimized influencing parameters on the extraction efficiency and morphology of the nanocomposite such as deposition potential, concentration of pyrrole and polyphosphate, deposition time and the nanosilica amount. Under the optimized conditions, characterization of the nanocomposite was inves-tigated by scanning electron microscopy and Fourier transform infra-red spectroscopy. Also, the factors related to the solid-phase microextraction method including desorption temperature and time, extrac-tion temperature and time, ionic strength and pH were studied in detail. Subsequently, the proposed method was validated by gas chromatography-mass spectrometry by thermal desorption and acceptable figures of merit were obtained. The linearity of the calibration curves was between 0.01 and 50 ng/mL with acceptable correlation coefficients (0.9956-0.9987) and limits of detection were in the range 0.002-0.01 ng/mL. Relative standard deviations in terms of intra-day and inter-day by five replicate analyses from aqueous solutions containing 0.1 ng/mL of target analytes were in the range 3.3%-5.4% and 5%-7.1%, respectively. Fiber-to-fiber reproducibilities were measured for three different fibers prepared in the same conditions and the results were between 7.3% and 9.8%. Also, extraction recoveries at two different concentrations were ≥96%. Finally, the suitability of the proposed method was demonstrated through its application to the analysis of some eye drops and injection solutions.

Covalent organic nanospheres as a fiber coating for solid-phase microextraction of genotoxic impurities followed by analysis using GC-MS

Covalent organic nanospheres(CONs)were explored as a fiber coating for solid-phase microextraction of genotoxic impurities(GTIs)from active ingredients(AIs).CONs were synthesized by an easy solutionphase procedure at 25℃.The obtained nanospheres exhibited a high specific surface area,good thermostability,high acid and alkali resistance,and favorable crystallinity and porosity.Two types of GTIs,alkyl halides(1-iodooctane,1-chlorobenzene,1-bromododecane,1,2-dichlorobenzene,1-bromooctane,1-chlorohexane,and 1,8-dibromooctane)and sulfonate esters(methyl p-toluenesulfonate and ethyl ptoluenesulfonate),were chosen as target molecules for assessing the performance of the coating.The prepared coating achieved high enhancement factors(5097-9799)for the selected GTIs.The strong affinity between CONs and GTIs was tentatively attributed to π-π and hydrophobicity interactions,large surface area of the CONs,and size-matching of the materials.Combined with gas chromatography-mass spectrometry(GC-MS),the established analytical method detected the GTIs in capecitabine and imatinib mesylate samples over a wide linear range(0.2-200 ng/g)with a low detection limit(0.04-2.0 ng/g),satisfactory recovery(80.03%-109.5%),and high repeatability(6.20%-14.8%)and reproducibility(6.20%-14.1%).Therefore,the CON-coated fibers are promising alternatives for the sensitive detection of GTIs in AI samples.

Solid-phase microextraction for flavor analysis in Harari Khat （Catha edulis） stimulant

This research examined the typical flavor compounds in the commonest type of Khat called Harari Khat grown in the region of Ethiopia.Twenty-eight compounds, which includes 1,2-Propanedione,1-Phenyl,Hexanol,Hexanal compounds,Limonene, Benzaldehyde with other flavors, were extracted by polydimethylsiloxane at room temperature for 30min from Khat samples,and identified by solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS).This method needs no organic solvents and required minimal sample.

Triacontyl modified silica gel as a sorbent for the preconcentration of polycyclic aromatic hydrocarbons in aqueous samples prior to gas chromatographic-mass spectrometry determination

Triacontyl modified silica gel as a sorbent coupled with gas chromatography-mass spectrometry(GC-MS) was developed to determine EPA prior 16 polycyclic aromatic hydrocarbons(PAHs) in water samples.Various parameters of solid-phase extraction such as organic modifier solvent,eluent,sample flow rate and volume were optimized.The developed method was found to yield a linear calibration curve in the concentration range of 0.05-8μg/L with respect to naphthalene,acenaphthylene,acenaphthene and 0.01-8μg/L for dibenz[a,h]anthracene and 0.05-14μg/L for fluorene,phenanthrene,anthracene and 0.01-14μg/L for the rest of analytes.Furthermore,the good accuracy and repeatability of the method made sure the requirements for achieving reliable analysis of PAHs in the environmental water samples,and the recoveries of optimal method were in the range of 80-120%except to higher volatility PAHs.C_(30)-bonded silica was proved to be an efficient sorbent for extraction of high molecular weight PAHs.

凝胶渗透色谱和气相色谱-质谱法测定动物食品中27种有机氯和15种拟除虫菊酯类农药残留量

A GC-MS method for the determination of 27 organochlorine pesticides and 15 Pyrethroid pesticides in animal food is established.The method was based on Gel Permeation chromatography combined with solid-phase extraction for sample preparation.Rapid qualitative and quantitative analyses was carried out by gas chromatography-mass spectrometry under the selective-ion monitoring mode.The experimental results showed that the correlation coefficients were better than 0.99,the recoveries for spiked standards were 70%-104%,the relative standard deviations were 2.1%-15.9%.

应用顶空-固相微萃取结合气相色谱-质谱联用技术分析传统锦州虾酱中挥发性物质

传统锦州虾酱是以白虾和乌虾为原料,在高盐条件下经长时间发酵形成海产风味食品。采用HPSPME/GC-MS结合保留指数方法分析虾酱中的挥发性物质,并对萃取条件进行优化。从DVB/PDMS、CAR/PDMS和DVB/CAR/PDMS筛选出最佳萃取头,同时采用正交试验优化SPME参数条件,确定适宜萃取条件为75μm CAR/PDMS萃取头,样品质量为5.0 g,萃取温度为70℃,萃取时间为50 min。对虾酱的风味物质分析得到44种挥发性物质,分别为醛类、酮类、酯类、酸类、酚类、烷烃类、吡嗪类和其他化合物。其中白虾虾酱主要呈香物质是醛类、吡嗪类和酚类等低阈值化合物,3-甲硫基丙醛、四甲基吡嗪和吲哚可能是白虾虾酱有别于乌虾虾酱的特有风味物质。乌虾虾酱主要呈香物质是醛类、酯类、酸类和酚类等低阈值化合物,酸类化合物是乌虾虾酱有别于白虾虾酱特有的风味物质,酯类化合物也可能是乌虾虾酱中风味物质的增味剂。

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。

玉米蛋白粉制备羊肉味风味料的工艺研究及风味成分分析

以玉米蛋白粉酶解液,控制氧化羊脂,D-木糖为主要原料,研究美拉德反应制备羊肉味风味料的最优工艺,并对羊肉味风味料的风味成分及可接受性进行分析。在单因素试验基础上,利用正交试验确定羊脂控制氧化的最优工艺及美拉德反应最佳反应条件;顶空固相微萃取-气相色谱质谱法(headspace solid-phase microextraction-gas chromatography-mass spectrometer,HS-SPME-GC-MS)测定羊肉味风味料的风味成分;模糊综合评价法确定了羊肉味风味料的可接受性。结果表明,羊脂控制氧化最优工艺为反应时间4. 0 h,温度135℃,通气量0. 30m^3/(kg·h);美拉德反应最佳反应条件为温度120℃,初始pH 6. 5,反应时间2 h;羊肉味风味料挥发性成分共检出24种风味物质,其中杂环类9种(88. 93%)、酸类6种(4. 98%)、酮类3种(0. 58%)、醛类2种(0. 61%)、酯类1种(0. 14%)、酚类1种(2. 12%)、胺类1种(0. 36%)(质量分数);模糊矩阵的综合评价结果表明人们对羊肉味风味料的喜欢比例为69%。

烤制时间对中式烤五花肉挥发性风味物质的影响

以猪五花肉为研究对象,利用万能蒸烤箱,研究恒定温度160℃条件下,不同烤制时间(5,10,15,20,25 min)对中式烤五花肉挥发性物质的影响。运用顶空固相微萃取(solid-phase microextraction,SPME)和气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)联用仪进行分析和鉴定,研究结果表明,中式烤五花肉在烤制时间下共鉴定出40种挥发性风味物质,其中醛类化合物7种、酯类化合物4种、醇类化合物8种、烃类化合物14种、其他化合物7种。从不同时间段来看,中式烤五花肉在烤制过程中,随着烤制时间的变化,在烤制25 min的条件下产生的挥发性物质数量最多。

Time-dependent categorization of volatile aroma compound formation in stewed Chinese spicy beef using electron nose profile coupled with thermal desorption GC–MS detection

In the present study,flavor profiles of Chinese spiced beef in the cooking process were comparatively analyzed by electronic nose,gas chromatography–mass spectrometry(GC–MS)with a thermal desorption system(TDS),and solid-phase microextraction(SPME).A total of 82 volatile compounds were identified,and 3-methyl-butanal,pentanal,hexanal,-xylene,heptanal,limonene,terpinene,octanal,linalool,4-terpinenol,-terpineol,and(E)-anethole were identified as the characteristic flavor compounds in Chinese spiced beef.Variation in the content of volatile components produced by different cooking processes was observed.In general,a cooking time of 4 h resulted in optimal flavor quality and stability.Results indicated that the electronic nose could profile and rapidly distinguish variation among different cooking time.The volatile profiling by TDS-GC–MS and responses from the electronic nose,in combination with multivariate statistical analysis,are a promising tool for control the cooking process of spiced beef.

Differential volatile organic compounds in royal jelly associated with different nectar plants

The aim of this work was to distinguish volatile organic compound（VOC） profiles of royal jelly（RJ） from different nectar plants. Headspace solid-phase microextraction（HS-SPME） was used to extract VOCs from raw RJ harvested from 10 nectar plants in flowering seasons. Qualitative and semi-quantitative analysis of VOCs extracts were performed by gas chromatography-mass spectrometry（GC-MS）. Results showed that VOC profiles of RJ from the samples were rich in acid, ester and aldehyde compound classes, however, contents of them were differential, exemplified by the data from acetic acid, benzoic acid methyl ester, hexanoic acid and octanoic acid. As a conclusion, these four VOCs can be used for distinguishing RJ harvested in the seasons of different nectar plants.

Determination of amphetamines,ketamine and their metabolites in hair with high-speed grinding and solid-phase microextraction followed by LC-MS

A novel hair sample pre-treatment method based on high-speed grinding and solid-phase microextraction(SPME)had been applied for the determination of amphetamines,ketamine and their metabolites in hair samples by liquid chromatography mass spectrometry(LC-MS).A 20mg sample of hair was ground with 2 mL of saturated sodium carbonate solution using a high-efficiency hair grinder with 70 Hz osillation for 2min at 4℃.After centrifuging,1.5mL of the supernatant was transferred and treated with SPME by direct immersion(DI-SPME).The target analytes extracted by fibre were desorbed and analysed using LC-MS.Under the optimum conditions,a recovery of 90.2%-95.8%was obtained for all analytes.The analytical method was linear for all analytes in the range from 0.2 to 10 ng/mg with the correlation coefficient ranging from 0.9985 to 0.9993.The detection limits for all analytes were estimated to be 0.067 ng/mg.The accuracy(mean relative error)was within±6.9%and the precision(relative standard error)was less than 6.8%.The combination of high-speed grinding of hair and SPME had the advantages of being easy to perform,environment-friendly and high in detection sensitivity.The proposed method offered an altermative ana lytical approach for the sensitive detection of drugs in hair samples for forensic purposes.

Eco-friendly and Cleaner Process Using Online Microwave-assisted Steam Extraction Coupled with Solid-phase Extraction for Trace Analysis of Sulfonamides in Animal Feed

An environmentally friendly method for extracting sulfonamides（SAs） residues from animal feed was described and applied. The method used online microwave-assisted steam extraction coupled with solid phase extraction（MASE-SPE）, which was followed by the analysis using high performance liquid chromatography-mass spectro- metry（HPLC-MS/MS）. The SAs residues were extracted successively with water steam under microwave irradiation, and thus directly introduced into an SPE colunm containing cation-exchange resin. The SAs were then eluted with methanol-ammonia（90：10, volume ratio） from the SPE column and followed by HPLC-MS/IVIS. The limits of detec- tion（LODs） for the analytes ranged from 0.24 ng/g to 0.49 ng/g. The limits of quantification（LOQs） ranged from 0.82 ng/g to 1.63 ng/g. Average recoveries of SAs were 76.3%--92.1%. The developed method was a reliable and envi-ronmentally friendly alternative to previous methods with respect to time, solvent and labor consumption for the analysis of SAs in animal foodstuffs.

Aroma changes of black tea prepared from methyl jasmonate treated tea plants

Methyl jasmonate（MeJA） was widely applied in promoting food quality.Aroma is one of the key indicators in judging the quality of tea.This study examined the effect of exogenous MeJA treatment on tea aroma.The aroma components in black tea prepared from MeJA-treated fresh tea leaves were extracted using headspace solid-phase microextraction（HS-SPME） and were analyzed using gas chromatography-mass spectrometry（GC-MS） and GC-olfactometry（GC-O）.Forty-five volatile compounds were identified.The results revealed that the MeJA-treated black tea had higher levels of terpene alcohols and hexenyl esters than the untreated tea.Moreover,several newly components,including copaene,cubenol,and indole,were induced by the MeJA treatment.The activities of polyphenol oxidase and β-glucosidase in fresh tea leaves changed after the MeJA treatment.Quantitative real-time polymerase chain reaction（qRT-PCR） analysis indicated that the gene expression levels of polyphenol oxidase and β-primeverosidase were upregulated by two and three folds,respectively,by the MeJA treatment（P0.01）; however,the gene expression of β-glucosidase was downregulated to a half level.In general,the aroma quality of the MeJAtreated black tea was clearly improved.

QSRR Study of GC Retention Indices of Volatile Compounds Emitted from Mosla chinensis Maxim by Multiple Linear Regression

The volatile compounds emitted from Mosla chinensis Maxim were analyzed by headspace solid-phase micro- extraction （HS-SPME） and headspace liquid-phase microextraction （HS-LPME） combined with gas chromatography-mass spectrometry （GC-MS）. The main volatiles from Mosla chinensis Maxim were studied in this paper. It can be seen that 61 compounds were separated and identified. Forty-nine volatile compounds were identified by SPME method, mainly including myrcene, a-terpinene, p-cymene, （E）-ocimene, thymol, thymol acetate and （E）-fl-farnesene. Forty-five major volatile compounds were identified by LPME method, including a-thujene, a-pinene, camphene, butanoic acid, 2-methylpropyl ester, myrcene, butanoic acid, butyl ester, a-terpinene, p-cymene, （E）-ocimene, butane, 1,1-dibutoxy-, thymol, thymol acetate and （E）-fl-farnesene. After analyzing the volatile compounds, multiple linear regression （MLR） method was used for building the regression model. Then the quantitative structure-retention relationship （QSRR） model was validated by predictive-ability test. The prediction results were in good agreement with the experimental values. The results demonstrated that headspace SPME-GC-MS and LPME-GC-MS are the simple, rapid and easy sample enrichment technique suitable for analysis of volatile compounds. This investigation provided an effective method for predicting the retention indices of new compounds even in the absence of the standard candidates.