In 2000 and 2001, 1-year-old seedlings of 7 economic tree species including chestnut, apricot, persimmon, peach, walnut, pear and apple were cultured in garden pots that had a diameter of 40 cm and were filled with cl...In 2000 and 2001, 1-year-old seedlings of 7 economic tree species including chestnut, apricot, persimmon, peach, walnut, pear and apple were cultured in garden pots that had a diameter of 40 cm and were filled with clean sand. The major components of exudates released from their roots were isolated and analysed by GC-MS. Totally 200 kinds of organic chemicals were isolated, of which 3 kinds i.e. naphthalene, dimethylbenzene and dibutyl phthalate were principally controlled pollutants according to 'Blacklist of Principal Environment Pollutants in China' and the standard of U.S. Environmental Protection Agency (EPA). The research result provided theoretical evidence for selecting low-pollution economic forest crops in the water source protection area in Miyun Reservoir.展开更多
An efficient analytical method combining pyrolysis and capillary GC/MS has been developed for determination and quantitation of targeted polycyclic aromatic hydrocarbons.The limit of detection ranged from 0.29 μg/g t...An efficient analytical method combining pyrolysis and capillary GC/MS has been developed for determination and quantitation of targeted polycyclic aromatic hydrocarbons.The limit of detection ranged from 0.29 μg/g to 43.46 μg/g,and repeatability values were between 0.1% and 8.2% for blank spiked samples and between 0.1 % and 9.8% for real samples of heavy oils.Through application of the proposed method in hydrotreating processes,it has been found out that heavy oils before and after the specified hydroprocessing treatment exhibited a diverse PAHs distribution which might be determined by the discrepancy in their intrinsic contents and hydrogenation reactivity.Furthermore,the hydrogenation reactivity of different polycyclic aromatic hydrocarbons was further investigated and discovered to be more interrelated to molecular structure and rings alignment or conjugation mode.展开更多
Phytoremediation effectiveness and remediation costs are driving factors of this project. Full utilization of plant resources after their being used for phytoremediation is an unsolved problem. GC/MS technique was use...Phytoremediation effectiveness and remediation costs are driving factors of this project. Full utilization of plant resources after their being used for phytoremediation is an unsolved problem. GC/MS technique was used to investigate the volatiles of the flowers from Elsholtzia argyi (PFE1: Purple Flower Elsholtzia) and their variation (WFE: White Flower Elsholtzia),naturally growing in Pb/Zn mined area, and Elsholtzia argyi (PFE2: Purple Flower Elsholtzia), naturally growing in Jiuxi uncontaminated agriculture soil. Seventeen compounds constituting 86.88% of total essential oils were identified in PFE1, with 2,6-octadienoic acid,3,7-dimethyl-methyl ester being the main constituent (63.30%). Sixteen compounds accounting for 95.32% of total essential oils were identified in WFE, with caryophyllene being the main component (55.02%). Compared to PFE1, PFE2 contained lower level of 2,6-octadienoic acid,3,7-dimethyl-methyl ester (31.76%), which was the main constituent in the total essential oils of PFE2. Caryophyllene is the main ingredient of flavor. Elsholtzia ketone was identified in all the three Elsholtzia plants. It can be concluded that the selected Elsholtzia argyi plants can be exploited on their versatile uses as fragrances and antiseptics due to the perfume ingredient and antibacterial components existing in their essential oils.展开更多
As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more effici...As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg^(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.展开更多
This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid e...This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.展开更多
Gas chromatography/mass spectrometry (GC MS) of the essential oil from the aerial parts of Rabdosia lophanthoides resulted in the identification of 108 compounds representing 78.120% of the oil. Hydro distillati...Gas chromatography/mass spectrometry (GC MS) of the essential oil from the aerial parts of Rabdosia lophanthoides resulted in the identification of 108 compounds representing 78.120% of the oil. Hydro distillation of Rabdosia lophanthoides yielded a pale yellow oil. The compounds identified and their relative proportions are listed in Table 1 according to their order of elution on an HP 5MS capillary column. .展开更多
For the purpose of obtaining small molecular and oxygen-containing aromatic compounds, taking a toluene-extracted coal pitch as the research object, the oxidation of coal-pitch by ozone （03） in formic acid was studi...For the purpose of obtaining small molecular and oxygen-containing aromatic compounds, taking a toluene-extracted coal pitch as the research object, the oxidation of coal-pitch by ozone （03） in formic acid was studied. The coal-pitch sample and the oxidized pitch residue were characterized by elementary analysis and Fourier transform infrared spectroscopy （FTIR）, while the small molecular products were analyzed by a gas chromatography-mass spectrometer （GC-MS）. The results show that the highest oxygen content of oxidized coal pitch had been acquired at a reaction temperature of 50℃C, an 03 flow rate of 6300 mg/h and a reaction time of 4 h. Quite a lot of hydroxyls and carbonyls were introduced into the structure of the oxidized coal-pitch, while the small molecules produced mainly involve nonpolar aro- matic compounds, aromatic anhydride and quinone compounds. It is speculated that the mechanism is direct electrophilic oxidation in which the molecules of 03 directly attack the aromatic ring at its carbon atoms with high electron density, and then generate hydroxyl or carbonyl until the aromatic ring cracks. This study shows that 03 can make the fused aromatic ring of coal-pitch become oxidized and depoly- merized, and hence the ozonization of coal-pitch can be a potential method for obtaining oxygen- containing aromatic compounds.展开更多
Mango fruit has a great national and international market, and Brazilian production is 1,900 thousand tons/year exporting to North America and Europe. However, the loss could occur during the production when it is aff...Mango fruit has a great national and international market, and Brazilian production is 1,900 thousand tons/year exporting to North America and Europe. However, the loss could occur during the production when it is affected by pests and climate conditions, so the increased use of chemical substances and their presence should be monitored. A task for governmental agencies, producers and food sales, attending the sanitary barriers requirements, is to distribute food free from contaminants, so laboratories involved in this type of work usually employ multi-residues analysis. The objective of this study was to evaluate the presence of pesticide residues in mango using QuEChERS method and mass spectrometry technique. Positive samples were compared with Brazilian maximum residues level （MRL） and the health risk exposure was evaluated using the acute dietary intake （ADI） parameter. A total of 20 samples were collected from January to March, in Sao Paulo city markets. The recoveries were in the range of 70% to 120%, and standard deviation was below 20%. The category of pesticides not permitted for the crop were found in l0 samples; eight samples presented pesticides below MRL and two samples above MRL for the fungicide procloraz. The ADI values were below 20% of ADI for an adult and the worst case was dimethoate with 69% of ADI for children. The time spent in monitoring studies and the viability of method chosen must be considered by pesticide residues laboratories during routine analysis of food quality control.展开更多
基金The study was supported by Natural Science Foundation of Beijing to Wang Yuzhu (No. 6992013).
文摘In 2000 and 2001, 1-year-old seedlings of 7 economic tree species including chestnut, apricot, persimmon, peach, walnut, pear and apple were cultured in garden pots that had a diameter of 40 cm and were filled with clean sand. The major components of exudates released from their roots were isolated and analysed by GC-MS. Totally 200 kinds of organic chemicals were isolated, of which 3 kinds i.e. naphthalene, dimethylbenzene and dibutyl phthalate were principally controlled pollutants according to 'Blacklist of Principal Environment Pollutants in China' and the standard of U.S. Environmental Protection Agency (EPA). The research result provided theoretical evidence for selecting low-pollution economic forest crops in the water source protection area in Miyun Reservoir.
基金support from the National Key Basic Research Science Foundation (Grant No. 2006CB202500. 4-1)
文摘An efficient analytical method combining pyrolysis and capillary GC/MS has been developed for determination and quantitation of targeted polycyclic aromatic hydrocarbons.The limit of detection ranged from 0.29 μg/g to 43.46 μg/g,and repeatability values were between 0.1% and 8.2% for blank spiked samples and between 0.1 % and 9.8% for real samples of heavy oils.Through application of the proposed method in hydrotreating processes,it has been found out that heavy oils before and after the specified hydroprocessing treatment exhibited a diverse PAHs distribution which might be determined by the discrepancy in their intrinsic contents and hydrogenation reactivity.Furthermore,the hydrogenation reactivity of different polycyclic aromatic hydrocarbons was further investigated and discovered to be more interrelated to molecular structure and rings alignment or conjugation mode.
文摘Phytoremediation effectiveness and remediation costs are driving factors of this project. Full utilization of plant resources after their being used for phytoremediation is an unsolved problem. GC/MS technique was used to investigate the volatiles of the flowers from Elsholtzia argyi (PFE1: Purple Flower Elsholtzia) and their variation (WFE: White Flower Elsholtzia),naturally growing in Pb/Zn mined area, and Elsholtzia argyi (PFE2: Purple Flower Elsholtzia), naturally growing in Jiuxi uncontaminated agriculture soil. Seventeen compounds constituting 86.88% of total essential oils were identified in PFE1, with 2,6-octadienoic acid,3,7-dimethyl-methyl ester being the main constituent (63.30%). Sixteen compounds accounting for 95.32% of total essential oils were identified in WFE, with caryophyllene being the main component (55.02%). Compared to PFE1, PFE2 contained lower level of 2,6-octadienoic acid,3,7-dimethyl-methyl ester (31.76%), which was the main constituent in the total essential oils of PFE2. Caryophyllene is the main ingredient of flavor. Elsholtzia ketone was identified in all the three Elsholtzia plants. It can be concluded that the selected Elsholtzia argyi plants can be exploited on their versatile uses as fragrances and antiseptics due to the perfume ingredient and antibacterial components existing in their essential oils.
基金supported by the National Natural Science Foundation of China (31071541)a program for Changjiang Scholars and Innovative Research Team in University (IRT1188)
文摘As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg^(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.
基金supported by the National Natural Science Foundation of China(41325010)
文摘This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.
文摘Gas chromatography/mass spectrometry (GC MS) of the essential oil from the aerial parts of Rabdosia lophanthoides resulted in the identification of 108 compounds representing 78.120% of the oil. Hydro distillation of Rabdosia lophanthoides yielded a pale yellow oil. The compounds identified and their relative proportions are listed in Table 1 according to their order of elution on an HP 5MS capillary column. .
基金financially supported by the Key Project of Science and Technology of Universities of Henan Province (No.14A530003)the Key Project of Science and Technology of Henan Province (No.152102310090)
文摘For the purpose of obtaining small molecular and oxygen-containing aromatic compounds, taking a toluene-extracted coal pitch as the research object, the oxidation of coal-pitch by ozone （03） in formic acid was studied. The coal-pitch sample and the oxidized pitch residue were characterized by elementary analysis and Fourier transform infrared spectroscopy （FTIR）, while the small molecular products were analyzed by a gas chromatography-mass spectrometer （GC-MS）. The results show that the highest oxygen content of oxidized coal pitch had been acquired at a reaction temperature of 50℃C, an 03 flow rate of 6300 mg/h and a reaction time of 4 h. Quite a lot of hydroxyls and carbonyls were introduced into the structure of the oxidized coal-pitch, while the small molecules produced mainly involve nonpolar aro- matic compounds, aromatic anhydride and quinone compounds. It is speculated that the mechanism is direct electrophilic oxidation in which the molecules of 03 directly attack the aromatic ring at its carbon atoms with high electron density, and then generate hydroxyl or carbonyl until the aromatic ring cracks. This study shows that 03 can make the fused aromatic ring of coal-pitch become oxidized and depoly- merized, and hence the ozonization of coal-pitch can be a potential method for obtaining oxygen- containing aromatic compounds.
文摘Mango fruit has a great national and international market, and Brazilian production is 1,900 thousand tons/year exporting to North America and Europe. However, the loss could occur during the production when it is affected by pests and climate conditions, so the increased use of chemical substances and their presence should be monitored. A task for governmental agencies, producers and food sales, attending the sanitary barriers requirements, is to distribute food free from contaminants, so laboratories involved in this type of work usually employ multi-residues analysis. The objective of this study was to evaluate the presence of pesticide residues in mango using QuEChERS method and mass spectrometry technique. Positive samples were compared with Brazilian maximum residues level （MRL） and the health risk exposure was evaluated using the acute dietary intake （ADI） parameter. A total of 20 samples were collected from January to March, in Sao Paulo city markets. The recoveries were in the range of 70% to 120%, and standard deviation was below 20%. The category of pesticides not permitted for the crop were found in l0 samples; eight samples presented pesticides below MRL and two samples above MRL for the fungicide procloraz. The ADI values were below 20% of ADI for an adult and the worst case was dimethoate with 69% of ADI for children. The time spent in monitoring studies and the viability of method chosen must be considered by pesticide residues laboratories during routine analysis of food quality control.
