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.

大鼠尿液中硝基安定代谢物的GC-MS检验

The metabolites and metabolic passways of nitrazepam in rat were confirmed.Wistar rats were feed a pill of nitrazepam,24 h urine reactions were collected.After β-Glucuronidase hydrolysis of the urine samples,the fractions were extracted by Oasis HLB3cc solid-phase column and analyzed by gas chromatography-mass spectrometry with DB-35 MS column.7-Acetylaminonitrazepam,7-aminonitrazepam and 2-amino-5-nitrophenylphenylmethanone were identified as nitrazepam metabolites.The results suggested that two metabolic passways for nitrazepam may be operative in rat.The first passway leads to the corresponding 7-aminonimetazepam in which the amino group is subsequently acetylated.The second passway is open the parent compounds rings to 2-amino-5-nitrophenylphenylmethanone.Nitrazepam was metabolized quickly in rats and 7-acetylaminonitrazepam were the main metabolites in urine.

气相色谱-负化学源质谱联用法测定水产品及食用油中氟乐灵的残留量

建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取，4℃冷藏后，采用分散型固相萃取法净化，由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证，同位素内标法定量。在1～40μg / L 范围内氟乐灵农药的线性关系良好；方法定量限（LOQ）为0.02μg / kg；对鳗鱼、烤鳗、梭子蟹、小龙虾、猪油和橄榄油等6种复杂基质进行1.0、2.0和3.0μg / kg 等3个水平的添加回收试验，平均回收率均处于80％～100％之间，RSD≤10.3％；无干扰现象出现。该方法可作为水产品及食用油中氟乐灵残留检测的确证方法。

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。

六种特级初榨橄榄油挥发性香气成分的比较

为探究比较特级初榨橄榄油挥发性香气成分,采用固相微萃取(solid phase micro-extraction,SPME)结合气相色谱嗅闻质谱(gas chromatography-olfactrometry-mass spectrometry,GC-O-MS)联用、感官评价和电子鼻技术对3个国家的6种特级初榨橄榄油挥发性香气成分进行分析。结果表明,电子鼻可以明显区分不同橄榄油;GC-O-MS通过极性色谱柱(DB-Wax)和非极性色谱柱(DB-5)结合分析,鉴定得出65种挥发性香气活性化合物,包括醛类16种,醇类12种,酯类9种,酮类6种,烯烃及萜烯类8种,芳香类5种,酸类3种及6种其他类型化合物。结合文献、检测及嗅闻结果得出特级初榨橄榄油中的特征香气成分为反-2-己烯醛、己醛、反-2-壬烯醛、6-甲基-5-庚烯-2-酮和顺-3-己烯-1-醇等以醛醇为代表的小分子化合物。

Analyses of BioVOCs variation related to vegetation predominance in the Natural Park of Ampezzo Dolomites, UNESCO world heritage area of Dolomites

The determination of emitted Biogenic Volatile Compounds （BioVOCs） profile via Field Air Analysis （FAA） - Solid Phase Micro Extraction （75μm Carboxen/PDMS portable field sampler） was performed using GC-MS. The six sampling sites located in the Natural Park of Ampezzo Dolomites, part of the UNESCO＇s World Heritage List, are characterized by different predominating vegetation. The ubiquitous compound hexanal was chosen as internal standard, in order to compare the amounts of the different compound in the different sites. The main terpenes identified were α-pinene, 13-pinene, 6-3-carene and d-limonene, while 1,8 cineole was the highest abundant oxygenated terpene. In the site next the＇national road a higher amount of benzene derivatives （ben- zene, toluene, o-xylene, p-xylene and ethylbenzene） were observed. In the site relatively close to the road a marked decrease of benzene deriva- tives was observed. In the sites close to conifers （i.e. Fir, Pine and Larch） the terpenic content observed was higher than in the site close to the mixed forest （mainly large-leaf and some conifers）. Some terpenes were observed also in the high-quote meadow site, although of lower abun- dance than in the other sites. The highest abundance of terpenes was ob- served in the Pinus cerebra （Swiss Pine） site.

Determination of Volatile Constituents,Total Flavonoids and Total Polysaccharides in the Roots of Artemisia argyi Levl. et Van. var.argyi cv. Qiai

[Objectives] To analyze the volatile components,the contents of total flavonoids and total polysaccharides of the roots of Artemisia argyi Levl. et Van. var. argyi cv. Qiai,and to provide a scientific basis for the comprehensive development and utilization of the resources.[Methods]The volatile components of the roots were extracted by solid phase micro-extraction( SPME),and its volatile components were analyzed by gas chromatography-mass spectrometry( GC-MS); the contents of total flavonoids and total polysaccharides in the samples were measured by UV-spectrophotometry. [Results] 44 peaks were isolated from the roots and 30 components were identified,accounting for 80. 9% of the total volatile components; the content of total flavonoids in the roots was 9. 42%; the content of total polysaccharides in the roots was 11. 05%.[Conclusions] After a comprehensive investigation,the olefins in the roots generally have antibacterial activity,the contents of the total flavonoids and total polysaccharides contained in the roots were relatively high,the roots of Artemisia argyi do have broad prospects for the development.

<i>Artemisia vulgaris</i>L. Chemotypes

Artemisia vulgaris L. was collected from various regions in the USA and Montreal Canada. Gas Chromatography-Mass Spectrometry was used to identify the analytes present in the volatiles extracted by headspace solid-phase microextraction of the crushed leaves and flowers. Four distinct chemotypes are were found: One featuring the coexistence of ar-curcumene and α-zingiberene;two marked by the presence or absence of thujone and santolinatriene;and a fourth characterized by the presence of crysanthenyl acetate (40%). DNA was used to confirm the identity of Artemisia vulgaris L.

Volatile Flavor Composition in Mutton of Ningxia Tan Sheep

[Objective] To analyze the volatile flavor compounds in mutton of different parts of Ningxia Tan sheep. [Method] The volatile flavor compounds in mutton were identified and quantified using the solid phase micro-extraction （SPME） method combined with GC-MS analysis. [ Re- sult ] The proportion of aldehydes in volatile compounds was the highest in the mutton of most parts of Ningxia Tan sheep, but no 4-methyl acid and 4-methyl nonyl acid was detected in the mutton. [ Conclusion]Aldehydes may be important for the volatile flavor of mutton of Ningxia Tan sheep. The study provides a basis for better development and use of Ningxia Tan sheep.

Effects of Grafting on Volatile Compounds in Bitter Gourd Fruit

[Objectives]This study was conducted to explore the effects of grafting on volatile compounds in bitter gourd fruit.[Methods]The volatile compounds and relative contents of grafted and non-grafted fruit were analyzed by headspace solid phase micro-extraction with gas chromatography-mass spectrometry.[Results]There were 59 volatile compounds in Haiyan No.2S,including six unique compounds.There were 58 volatile compounds in Haiyan No.2J,including five unique compounds.[Conclusions]This study provides a scientific basis for further analysis of bitter gourd flavor regulation mediated by grafting.

The impact of a Wastewater Treatment Works in Southern Gauteng, South Africa on efavirenz and nevirapine discharges into the aquatic environment

There has been growing concern regarding the pollution of the aquatic environment with synthetic organic chemicals.Antiretroviral drugs,such as efavirenz and nevirapine,are pharmaceutical drugs and are referred to as emerging contaminants.Such drugs can be environmentally persistent and may be expected to pose potential risks to drinking water supplies.Sources of pharmaceutical drugs include effluents from Wastewater Treatment Works(WWTPs),hospital and pharmaceutical production facilities and the incorrect disposal of unused and expired medicines.Currently there are no monitoring programs and legislative guidelines for their regulations in South Africa.The aims of this study were firstly to develop a semi-quantitative method to extract and analyse efavirenz and nevirapine in the primary settling tank sludge.Secondly to use that method,and an existing method for liquid wastewater samples,to monitor the concentrations of efavirenz and nevirapine as the wastewater passes through the different stages of purification(anoxic;aerobic;pre and post chlorination)in the WWTP.This was repeated weekly over a period of 4 weeks.Thirdly,to determine if binding of efavirenz and nevirapine to the solids in the WWTP played a role in the removal of these compounds from the WWTP liquid phase.No references to the analysis of ARVDs in WWTP sludge were found in the literature.Grab samples of wastewater and sludge samples were collected from a WWTP(activated sludge treatment process)weekly for 4 weeks.Liquid samples were extracted solid phase extraction,solid samples were extracted using sonication followed by a QuEChERs clean-up.Sample extracts were then subjected to gas chromatography-time of flight mass spectrometry for analyte determination.Efavirenz concentrations entering the WWTP ranged between 5500 to almost 14000 ng/L.The removal of efavirenz by the WWTP ranged between 27 and 71%.The largest removal occurred in the anoxic zone,smaller amounts were removed in the aerators.Slight increases in efavirenz concentrations were found after chlorination and the final effluent into the river post maturation ponds again were slightly lower.Solids were found to contain efavirenz at concentrations between 17 and 43 mg/kg dried primary settling tank sludge and it is proposed that this binding to the solids is the main mechanism of removal of efavirenz from the wastewater stream as it passes through the WWTP.Although an order of magnitude lower nevirapine concentrations displayed the opposite behaviour and gradually increased through the various stages of purification in the WWTP.Minor fluctuations occurred but the concentrations of nevirapine were higher at the effluent(between 92 and 473 ng/L)than those entering the WWTP.No nevirapine was detected in the PST sludge.The increase in nevirapine concentrations are likely to be the result of the de-conjugation of the hydroxylated metabolites of nevirapine in the WWTP,its resistance to degradation and the lack of binding of the nevirapine to the PST sludge.

Developing an authentication approach using SPME-GC-IRMS based on compound-specific δ^(13)C analysis of six typical volatiles in wine

An analytical method using gas chromatography isotope ratio mass spectrometry(GC-IRMS)combined with solid phase micro-extraction(SPME)was developed to measure the 613C values of six typical volatiles commonly occurring in wine(isoamyl acetate,2-octanone,limonene,2-phenylethanol,ethyl octanoate and ethyl decanoate)for the first time.SPME selected with a divinylbenzene/carboxen/polydimethylsiloxane fiber was combined with the GC-IRMS for pretreatment optimization.The optimized SPME parameters of extraction time,extraction temperature and salt concentration were 40 min,40℃ and 10%,respectively.The 613C values measured by SPME-GC-IRMS were in good agreement with those measured via elemental analyzer(EA)-IRMS and GC-IRMS.The differences range from 0.02‰to 0.44‰ with EA-IRMS and from 0 to 0.28‰ with GC-IRMS,indicating the high accuracy of the method.This newly established method measured the precision within 0.30‰ and was successfully validated to discriminate imported real wine samples with identical label but amazing price differences from different importers.

Estimation of the Postmortem Interval Using Chromatographic Fingerprints of Volatile Organic Compounds from Muscle

Estimation of the postmortem interval(PMI)is a crucial task in the field of forensic pathology and has unfortunately not been properly resolved.In this study,we analyzed volatile organic compounds(VOCs)in rat muscle samples collected at different PMIs and studied the feasibility of muscle VOC fingerprinting as a new method for PMI estimation.In total,110 rats were sacrificed and stored at a constant temperature(25℃).Rat skeletal muscle samples were collected at 0-10‑day postmortem,and then the VOCs were determined using a method of headspace solid‑phase microextraction coupled with gas chromatography‑mass spectrometry.The correlations between the VOCs(species and quantities)and PMIs were carefully analyzed and standard muscle VOC fingerprints at 25℃were established for different PMIs.To further test the accuracy of muscle VOC fingerprinting as a method for PMI estimation,ten additional rats with known PMIs were studied.We identified 15 kinds of VOCs and the number of VOC species increased with the PMI.The total peak areas of the VOCs increased significantly with the postmortem day(adjusted R^(2)=0.96-0.97).The mean error of the VOC fingerprinting for PMI estimation was 0.5 days and the mean relative error was 8.33%.We concluded that muscle VOC fingerprinting combining the use of VOC species and peak areas is accurate and effective and could be used as an alternative approach for PMI estimation in forensic practice.Although the preliminary results are encouraging,further studies in human cadavers under real case conditions are needed.