Gas chromatographymass spectrometry (GC-MS) coupled with chemometric resolution upon two- dimensional data was employed to analyze the constituents of essential oils of Angelica sinensis. Constituents in essential oil...Gas chromatographymass spectrometry (GC-MS) coupled with chemometric resolution upon two- dimensional data was employed to analyze the constituents of essential oils of Angelica sinensis. Constituents in essential oils of Angelica sinensis root were identified by GC-MS with the help of subwindow factor analysis (SFA) method resolving two-dimensional original data into mass spectra and chromatograms. 76 of 97 separated constituents in essential oil of Angelica sinensis root were identified and quantified, and they account for about 91.36% of the total content. The results show that ligustilide, butylene phthalide, 2-methoxy-4-vinylphenol, carvacrol, allo-ocimene,2,6,6-trimethylbicyclo-[3,1,1]hept-2-ene are the main constituents in essential oil of Angelica sinensis root.展开更多
The flammability characterization and thermal composition of polymers flame retarded by decabromodiphenylethane (DBDPE) and antimony trioxide (Sb2O3) were studied by cone calorimeter and thermogravimetry (TG). The res...The flammability characterization and thermal composition of polymers flame retarded by decabromodiphenylethane (DBDPE) and antimony trioxide (Sb2O3) were studied by cone calorimeter and thermogravimetry (TG). The results show that ABS/DBDPE/Sb2O3 has the similar flammability parameters and thermal composition curves to ABS/DBDPO/Sb2O3. It suggests that DBDPE/Sb2O3 has the similar flame retardant behavior to DBDPO/Sb2O3. The heat release rate (HRR) and the effect heat combustion (EHC) curves of polymers flame retarded by DBDPE/Sb2O3 all decrease, but the mass loss rate (MLR) curve slightly increase. It shows that the decrease of HRR is not due to the increase of char formation ratio but the generation of incombustible gases. The major flame retardant mechanism of DBDPE/Sb2O3 is gas phase flame retardant mechanism. Increasing content of Sb2O3 in DBDPE/Sb2O3 can improve the flame retardant property and thermal stability of acrylonitrile butadiene styrene. Sb2O3 has a good synergistic effect with DBDPE.展开更多
Codfish is a kind of abyssal fish species with a great value in food industry. However, the flavor of codfish, especially the unpleasant odor, has caused serious problems in its processing. To accurately identify the ...Codfish is a kind of abyssal fish species with a great value in food industry. However, the flavor of codfish, especially the unpleasant odor, has caused serious problems in its processing. To accurately identify the volatile compounds in codfish, a combination of solid phase micro-extraction(SPME) method and simultaneous distillation extraction(SDE) method was used to extract the volatiles. Gas chromatography-mass spectrometry(GC-MS) along with Kovats indices(KI) and authentic standard compounds were used to identify the volatiles. The results showed that a total of 86 volatile compounds were identified in codfish, of them 24 were extracted by SDE, 69 compounds by SPME, and 10 compounds by both SDE and SPME. Seventy volatile compounds were found to have specific odors, of them 7 typical compounds contributed significantly to the flavor of codfish. Alcohols(i.e.,(E)-2-penten-1-ol and 2-octanol), esters(i.e., ethyl butyrate and methyl geranate), aldehydes(i.e., 2-dodecenal and pentadecanal) contributed the most to fresh flavor while nitrogen compounds, sulphur compounds, furans, as well as some ketones(i.e., 2-hydroxy-3-pentanone) brought unpleasant odor, such as fishy and earthy odor. It was indicated that the combination of multiple extraction methods and GC-MS analysis can enhance the accuracy of identification, and provide a reference for the further study on flavor of aquatic products.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
Biodiesel bioremediation in soils may occur by natural attenuation or by engineered techniques, such as biostimulation and bioaugmentation. The present study evaluated the degradation of biodiesel in two soils with di...Biodiesel bioremediation in soils may occur by natural attenuation or by engineered techniques, such as biostimulation and bioaugmentation. The present study evaluated the degradation of biodiesel in two soils with different particle size characteristics by the bioremediation processes of natural attenuation and biostimulation. The experiment was carried out ex situ, with the factors temperature, moisture content, and pH being controlled for the experimental period of 110 days. The study aimed at evaluating the biodegradation of a clayey soil (A) and a sandy soil (B), both contaminated with pure biodiesel, by using the analytical methods of respirometry and gas chromatography. Biostimulation treatments using nitrogen, phosphorus, and potassium solutions (NPK) promoted higher microbiological activity in both soils. At the end of the experiment, it was observed that biostimulation was more efficient when compared to natural attenuation, showing higher biodiesel degradation for both soils A (59.76%) and B (90.41%).展开更多
Discrimination of fatty acids (FAs) of lard in used cooking oil is important in halal determination. The aim of this study was to find the information related to the changes FAs of lard when frying in cooking oil. Q...Discrimination of fatty acids (FAs) of lard in used cooking oil is important in halal determination. The aim of this study was to find the information related to the changes FAs of lard when frying in cooking oil. Quantitative analysis of FAs composition extracted from a series of experiments which involving frying cooking oil spiked with lard at three different parameters; concentration of spiked lard, heating temperatures and period of frying. The samples were analyzed using Gas Chromatography (GC) and Principal Components Analysis (PCA) technique. Multivariate data from chromatograms of FAs were standardized and computed using Unscrambler X10 into covariance matrix and eigenvectors correspond to Principal Components (PCs). Results have shown that the first and second PCs contribute to the FAs mapping which can be visualized by scores and loading plots to discriminate FAs of lard in used cooking oil展开更多
Dynamic characteristics of UV enhanced gas–solid PVC chlorination process were revealed by a UV–Vis spectral online analysis method. Experimental results showed an instantaneous increase of the chlorination rate as ...Dynamic characteristics of UV enhanced gas–solid PVC chlorination process were revealed by a UV–Vis spectral online analysis method. Experimental results showed an instantaneous increase of the chlorination rate as soon as UV light was affiliated, which demonstrated the intensified effect of UV radiation on PVC chlorination directly.Different affiliation methods of UV light were then studied, proving that continuous UV radiation could enhance the chlorination process significantly while intermittent UV radiation was able to initiate the chlorination reaction once it was conducted. Besides, experiments were carried out to study the influences of parameters on the chlorination process such as UV wavelength, chlorination temperature, partial pressure of chlorine gas and PVC raw materials. Among all the parameters, chlorination temperature and partial pressure of chlorine gas were testified as two key factors to determine the chlorination performance. Thermal analysis of CPVC products showed that their corresponding properties such as the glass transition temperature(Tg) and the homogeneity of chlorine distribution in polymer phase were improved with the increase of chlorine content.展开更多
The pyrolysis of different waste polymers (polyethylene, polypropylene and polystyrene) was investigated in a tube reactor at 550 ℃ in the absence of oxygen. Additionally the energetic utilization of products have ...The pyrolysis of different waste polymers (polyethylene, polypropylene and polystyrene) was investigated in a tube reactor at 550 ℃ in the absence of oxygen. Additionally the energetic utilization of products have also been followed both in refining and petrochemical industry. Pyrolysis products were separated into fractions of gases, naphtha, middle distillates and heavy oil. Raw materials have been collected both from industrial and household sources: polyethylene from agriculture, polyethylene from packaging and polystyrene from packaging and electronic equipments. Yields and properties of volatile products have changed by the raw materials. Products have been analyzed by gas chromatography. Fourier transformed infrared spectroscopy, size exclusion chromatography and other standardized methods. Naphtha had high octane numbers (80 〈 RON), while high cetane numbers (〉 75) in case of middle distillates. Moreover fractions contained approximately half of unsaturated hydrocarbons, mainly α-olefins, but the percentage was depending on the raw materials. These properties are advantageous for fuel-like applications.展开更多
Currently, biodiesel is presented as one of the best alternatives for gradually replacing the use of fossil fuels, but it has some factors that make it economically impractical if it does not have a government support...Currently, biodiesel is presented as one of the best alternatives for gradually replacing the use of fossil fuels, but it has some factors that make it economically impractical if it does not have a government support. For this reason, research efforts focused on this area have been responsible for optimizing the process of biodiesel production by different catalytic routes to achieve greater efficiency at a lower cost. In this case, the biggest problem has been the high cost generated by an investigation, which in many occasions is the main factor to decide if an investigation could be carried out. Trying to reduce these costs, in the current study, we are using a technique of glycerol quantification by volumetric methods and comparing obtained results with the chromatographic method, which is conventionally used and comparatively much more expensive. Biodiesel employee was obtained by an enzymatic catalysis process varying one of three process variables:oil:alcohol molar ratio, temperature and proportion of catalyst. The numerical differences obtained between the two quantification methods generated relative errors lower than 10%, resulting in some occasions lower than 1%. By gas chromatography analysis the best yield was obtained at the same conditions of the volumetric method, a temperature of 45 ℃, an oil:alcohol ratio 1:4 and 8 wt.% of catalyst, but a yield of 95.5% and 97.1%, respectively. Due to the high precision of gas chromatography, this method is used to carry out a surface response analysis obtaining as ideal operating conditions a temperature of 43.5 ℃, 8.9 wt.%. of catalyst and an oil:alcohol ratio 1:4.展开更多
Pesticides have done a great service to human, but their use is not safe for public health. Apart from pesticides acute toxicity, their chronic toxicity can cause various problems for human health. The objective of th...Pesticides have done a great service to human, but their use is not safe for public health. Apart from pesticides acute toxicity, their chronic toxicity can cause various problems for human health. The objective of this work was to validate a liquid-liquid extraction method, which allows a fairly reliable analysis of pesticides using gas chromatography-spectrometry mass (GC/MS) in toxicology laboratory at National Institute of hygiene, Rabat Morocco. The equipment required to perform these analyzes are the biological matrices (blood, gastric fluid), in which the authors have doped the Organophosphorus pesticides such as Chlorpyrifos, Dichlorvos and Organochlorine pesticide: dichlorodiphenyltrichloroethane (DDT) and Heptachlor. After extracting the mixture with toluene, the supernatant was collected after centrifugation and concentrated in a small volume of 1.5 mL and then analyzed in GC/MS. After analyzing, the authors found that the yields of each pesticide in samples are significant; respectively they represented 73.4% of Chlorpyrifos, 70.8% of Dichlorvos, 47.8% of DDT and 71.6% of Heptachlor. The blood has a strong link with the most pesticides, where it's important to use the GC/MS to identify these products. The extraction with toluene was effective, especially to OP, but it's also sensitive to OC.展开更多
文摘Gas chromatographymass spectrometry (GC-MS) coupled with chemometric resolution upon two- dimensional data was employed to analyze the constituents of essential oils of Angelica sinensis. Constituents in essential oils of Angelica sinensis root were identified by GC-MS with the help of subwindow factor analysis (SFA) method resolving two-dimensional original data into mass spectra and chromatograms. 76 of 97 separated constituents in essential oil of Angelica sinensis root were identified and quantified, and they account for about 91.36% of the total content. The results show that ligustilide, butylene phthalide, 2-methoxy-4-vinylphenol, carvacrol, allo-ocimene,2,6,6-trimethylbicyclo-[3,1,1]hept-2-ene are the main constituents in essential oil of Angelica sinensis root.
基金Project(20574020) supported by the National Natural Science Foundation of China
文摘The flammability characterization and thermal composition of polymers flame retarded by decabromodiphenylethane (DBDPE) and antimony trioxide (Sb2O3) were studied by cone calorimeter and thermogravimetry (TG). The results show that ABS/DBDPE/Sb2O3 has the similar flammability parameters and thermal composition curves to ABS/DBDPO/Sb2O3. It suggests that DBDPE/Sb2O3 has the similar flame retardant behavior to DBDPO/Sb2O3. The heat release rate (HRR) and the effect heat combustion (EHC) curves of polymers flame retarded by DBDPE/Sb2O3 all decrease, but the mass loss rate (MLR) curve slightly increase. It shows that the decrease of HRR is not due to the increase of char formation ratio but the generation of incombustible gases. The major flame retardant mechanism of DBDPE/Sb2O3 is gas phase flame retardant mechanism. Increasing content of Sb2O3 in DBDPE/Sb2O3 can improve the flame retardant property and thermal stability of acrylonitrile butadiene styrene. Sb2O3 has a good synergistic effect with DBDPE.
基金supported by the National Natural Science Foundation of China (Nos. 31401476, 31471606)National High-Tech Research and Development Program of China, 863 Program (2014AA093508)Shandong Province Regional Innovation and Development of Marine Economy Demonstration Project
文摘Codfish is a kind of abyssal fish species with a great value in food industry. However, the flavor of codfish, especially the unpleasant odor, has caused serious problems in its processing. To accurately identify the volatile compounds in codfish, a combination of solid phase micro-extraction(SPME) method and simultaneous distillation extraction(SDE) method was used to extract the volatiles. Gas chromatography-mass spectrometry(GC-MS) along with Kovats indices(KI) and authentic standard compounds were used to identify the volatiles. The results showed that a total of 86 volatile compounds were identified in codfish, of them 24 were extracted by SDE, 69 compounds by SPME, and 10 compounds by both SDE and SPME. Seventy volatile compounds were found to have specific odors, of them 7 typical compounds contributed significantly to the flavor of codfish. Alcohols(i.e.,(E)-2-penten-1-ol and 2-octanol), esters(i.e., ethyl butyrate and methyl geranate), aldehydes(i.e., 2-dodecenal and pentadecanal) contributed the most to fresh flavor while nitrogen compounds, sulphur compounds, furans, as well as some ketones(i.e., 2-hydroxy-3-pentanone) brought unpleasant odor, such as fishy and earthy odor. It was indicated that the combination of multiple extraction methods and GC-MS analysis can enhance the accuracy of identification, and provide a reference for the further study on flavor of aquatic products.
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.
文摘Biodiesel bioremediation in soils may occur by natural attenuation or by engineered techniques, such as biostimulation and bioaugmentation. The present study evaluated the degradation of biodiesel in two soils with different particle size characteristics by the bioremediation processes of natural attenuation and biostimulation. The experiment was carried out ex situ, with the factors temperature, moisture content, and pH being controlled for the experimental period of 110 days. The study aimed at evaluating the biodegradation of a clayey soil (A) and a sandy soil (B), both contaminated with pure biodiesel, by using the analytical methods of respirometry and gas chromatography. Biostimulation treatments using nitrogen, phosphorus, and potassium solutions (NPK) promoted higher microbiological activity in both soils. At the end of the experiment, it was observed that biostimulation was more efficient when compared to natural attenuation, showing higher biodiesel degradation for both soils A (59.76%) and B (90.41%).
文摘Discrimination of fatty acids (FAs) of lard in used cooking oil is important in halal determination. The aim of this study was to find the information related to the changes FAs of lard when frying in cooking oil. Quantitative analysis of FAs composition extracted from a series of experiments which involving frying cooking oil spiked with lard at three different parameters; concentration of spiked lard, heating temperatures and period of frying. The samples were analyzed using Gas Chromatography (GC) and Principal Components Analysis (PCA) technique. Multivariate data from chromatograms of FAs were standardized and computed using Unscrambler X10 into covariance matrix and eigenvectors correspond to Principal Components (PCs). Results have shown that the first and second PCs contribute to the FAs mapping which can be visualized by scores and loading plots to discriminate FAs of lard in used cooking oil
基金Supported by the National Science and Technology Key Supporting Project(2013BAF08B05)the National Natural Science Foundation of China(21176137)
文摘Dynamic characteristics of UV enhanced gas–solid PVC chlorination process were revealed by a UV–Vis spectral online analysis method. Experimental results showed an instantaneous increase of the chlorination rate as soon as UV light was affiliated, which demonstrated the intensified effect of UV radiation on PVC chlorination directly.Different affiliation methods of UV light were then studied, proving that continuous UV radiation could enhance the chlorination process significantly while intermittent UV radiation was able to initiate the chlorination reaction once it was conducted. Besides, experiments were carried out to study the influences of parameters on the chlorination process such as UV wavelength, chlorination temperature, partial pressure of chlorine gas and PVC raw materials. Among all the parameters, chlorination temperature and partial pressure of chlorine gas were testified as two key factors to determine the chlorination performance. Thermal analysis of CPVC products showed that their corresponding properties such as the glass transition temperature(Tg) and the homogeneity of chlorine distribution in polymer phase were improved with the increase of chlorine content.
文摘The pyrolysis of different waste polymers (polyethylene, polypropylene and polystyrene) was investigated in a tube reactor at 550 ℃ in the absence of oxygen. Additionally the energetic utilization of products have also been followed both in refining and petrochemical industry. Pyrolysis products were separated into fractions of gases, naphtha, middle distillates and heavy oil. Raw materials have been collected both from industrial and household sources: polyethylene from agriculture, polyethylene from packaging and polystyrene from packaging and electronic equipments. Yields and properties of volatile products have changed by the raw materials. Products have been analyzed by gas chromatography. Fourier transformed infrared spectroscopy, size exclusion chromatography and other standardized methods. Naphtha had high octane numbers (80 〈 RON), while high cetane numbers (〉 75) in case of middle distillates. Moreover fractions contained approximately half of unsaturated hydrocarbons, mainly α-olefins, but the percentage was depending on the raw materials. These properties are advantageous for fuel-like applications.
文摘Currently, biodiesel is presented as one of the best alternatives for gradually replacing the use of fossil fuels, but it has some factors that make it economically impractical if it does not have a government support. For this reason, research efforts focused on this area have been responsible for optimizing the process of biodiesel production by different catalytic routes to achieve greater efficiency at a lower cost. In this case, the biggest problem has been the high cost generated by an investigation, which in many occasions is the main factor to decide if an investigation could be carried out. Trying to reduce these costs, in the current study, we are using a technique of glycerol quantification by volumetric methods and comparing obtained results with the chromatographic method, which is conventionally used and comparatively much more expensive. Biodiesel employee was obtained by an enzymatic catalysis process varying one of three process variables:oil:alcohol molar ratio, temperature and proportion of catalyst. The numerical differences obtained between the two quantification methods generated relative errors lower than 10%, resulting in some occasions lower than 1%. By gas chromatography analysis the best yield was obtained at the same conditions of the volumetric method, a temperature of 45 ℃, an oil:alcohol ratio 1:4 and 8 wt.% of catalyst, but a yield of 95.5% and 97.1%, respectively. Due to the high precision of gas chromatography, this method is used to carry out a surface response analysis obtaining as ideal operating conditions a temperature of 43.5 ℃, 8.9 wt.%. of catalyst and an oil:alcohol ratio 1:4.
文摘Pesticides have done a great service to human, but their use is not safe for public health. Apart from pesticides acute toxicity, their chronic toxicity can cause various problems for human health. The objective of this work was to validate a liquid-liquid extraction method, which allows a fairly reliable analysis of pesticides using gas chromatography-spectrometry mass (GC/MS) in toxicology laboratory at National Institute of hygiene, Rabat Morocco. The equipment required to perform these analyzes are the biological matrices (blood, gastric fluid), in which the authors have doped the Organophosphorus pesticides such as Chlorpyrifos, Dichlorvos and Organochlorine pesticide: dichlorodiphenyltrichloroethane (DDT) and Heptachlor. After extracting the mixture with toluene, the supernatant was collected after centrifugation and concentrated in a small volume of 1.5 mL and then analyzed in GC/MS. After analyzing, the authors found that the yields of each pesticide in samples are significant; respectively they represented 73.4% of Chlorpyrifos, 70.8% of Dichlorvos, 47.8% of DDT and 71.6% of Heptachlor. The blood has a strong link with the most pesticides, where it's important to use the GC/MS to identify these products. The extraction with toluene was effective, especially to OP, but it's also sensitive to OC.