A trace analytical method based on solid-phase extraction gas chromatography-tandem mass spectrometry(SPE–GC–MS/MS)was developed for the rapid detection of 256 semi-volatile organic compounds(SVOCs),including 25 pol...A trace analytical method based on solid-phase extraction gas chromatography-tandem mass spectrometry(SPE–GC–MS/MS)was developed for the rapid detection of 256 semi-volatile organic compounds(SVOCs),including 25 polycyclic aromatic hydrocarbons(PAHs),70 polychlorinated biphenyls(PCBs),123 pesticides,20 phthalate esters(PAEs),4 organophosphate esters(OPEs),9 synthetic musks(SMs),and 5 UV filters(UVs)in water.No-tably,this method provided a decent linearity of calibration standards(R^(2)>0.999),excellent method limits of quantification(MLOQs)(0.12–11.41 ng/L),satisfactory matrix spiking recovery rates(60.4%–126%),and high precision(intra-day relative standard deviations(RSDs):1.0%–10.0%,inter-day RSDs:3.0%–15.0%,and inter-week RSDs:3.4%–15.7%),making it suitable for trace-level studies.Statistical analysis revealed that SVOCs with higher volatility exhibited enhanced recovery rates.Validation of the methodology involved analyzing SVOCs in real spring water and river water samples.Twenty-seven SVOCs were detected in spring water and 58 in river water,with an average concentration of 631.73 and 16,095 ng/L,respectively.Among the detected SVOCs,PAEs constituted the predominant proportion.This study underscored the presence of SVOCs contamination specifi-cally within the spring water,although SVOCs concentrations in river water were significantly greater than those found in spring water.In summary,this sensitive method based on SPE–GC–MS/MS was successfully developed and validated for the rapid analysis of a diverse array of 256 SVOCs at trace levels in water,including not only the traditional highly valued PAHs,PCBs,pesticides,and PAEs,but also the emerging OPEs,UVs,and SMs.展开更多
[Objective] This study was aimed to determine the optimal parameters for the extraction of perilla seed oil to obtain high-quality perilla seed oil and analyze its compositions. [Method] In this study, perilla seed oi...[Objective] This study was aimed to determine the optimal parameters for the extraction of perilla seed oil to obtain high-quality perilla seed oil and analyze its compositions. [Method] In this study, perilla seed oil was extracted using supercritical CO2 （SC-CO2）. The effects of extraction time, temperature and pressure were investigated by single-factor experiments and orthogonal array testing （ORT）. The chemical compositions of extracted perilla seed oil were investigated by GC-MS. [Result] The optimal conditions for the extraction of perilla seed oil using SC-CO2 were extraction time of 4 h, extraction temperature at 40 ℃, and extraction pressure at 23 MPa. Under these conditions, the extraction yield of perilla seed oil was maximized to 12.43%. GC-MS analysis revealed that perilla seed oil was a complex mixture containing 76.183% α-linolenic acid. [Conclusion] Supercritical CO2 extraction was proven to be an effective technology to extract oil from perilla seed, and GCMS was also a satisfactory method for analyzing the compositions of perilla seed oil.展开更多
To determine the chemical constituents of volatile components in saffron from the Tibet Autonomous Region and the Henan Province of China and to compare the chemical composition difference in the saffron,the total vol...To determine the chemical constituents of volatile components in saffron from the Tibet Autonomous Region and the Henan Province of China and to compare the chemical composition difference in the saffron,the total volatile components were extracted by ultrasonic-assisted solvent extraction（USE）,using five different solvents：diethyl ether,ethanol,ethyl acetate, dichloromethane and acetone,analyzed using gas chromatography-mass spectrometry（GC-MS）and compared to the standard MS data,and their relative contents were calculated by area normalization.The results showed both that USE was an efficient and rapid method for the extraction of the volatile components from saffron and that the components extracted from the same sample using different solvents were different.Comparison of the experimental results of saffron from the Tibet Autonomous Region and the Henan Province of China showed that their volatile components were different in their chemical composition and in their relative percentages.USE/GC-MS is a simple,rapid,and effective method for the analysis of volatile oil components in saffron.展开更多
Background:Cyperi Rhizoma,derived from Cyperus rotundus L.,is a widely used medicinal herb in traditional Chinese medicine(TCM),with Shandong Province recognized as its geo-authentic habitat.However,the quality of Cyp...Background:Cyperi Rhizoma,derived from Cyperus rotundus L.,is a widely used medicinal herb in traditional Chinese medicine(TCM),with Shandong Province recognized as its geo-authentic habitat.However,the quality of Cyperi Rhizoma varies significantly across different regions,potentially influencing its therapeutic efficacy.This study investigates the influence of geographic origin on the chemical composition and overall quality of Cyperi Rhizoma.Methods:A comprehensive approach,including traditional quality assessment,GC-MS(g as c hromatography-m ass s pectrometry),RP-HPLC(r everse p hase h igh-p erformance l iquid c hromatography),and FT-IR(f ourier t ransform i nfrared s pectroscopy)techniques,was employed to analyze Cyperi Rhizoma samples from Shandong Province.These methods examined the physical appearance,chemical profile,and content variations,particularly focusing onα-cyperone.Results:Traditional quality assessments revealed noticeable differences in the external characteristics of the samples.GC-MS analysis identified a variety of unique chemical constituents,while RP-HPLC and FT-IR showed significant variations inα-cyperone content,with higher levels found in Shandong samples.Conclusion:These results demonstrate that geographic origin is a critical determinant of Cyperi Rhizoma quality,with Shandong specimens exhibiting superiorα-cyperone levels and characteristic phytochemical profiles.This validates the geo-authenticity concept in TCM and provides actionable data for developing evidence-based quality standards,suggesting that provenance should be prioritized in medicinal material selection and pharmacopeial specifications.展开更多
Since Google introduced the concept of Knowledge Graphs(KGs)in 2012,their construction technologies have evolved into a comprehensive methodological framework encompassing knowledge acquisition,extraction,representati...Since Google introduced the concept of Knowledge Graphs(KGs)in 2012,their construction technologies have evolved into a comprehensive methodological framework encompassing knowledge acquisition,extraction,representation,modeling,fusion,computation,and storage.Within this framework,knowledge extraction,as the core component,directly determines KG quality.In military domains,traditional manual curation models face efficiency constraints due to data fragmentation,complex knowledge architectures,and confidentiality protocols.Meanwhile,crowdsourced ontology construction approaches from general domains prove non-transferable,while human-crafted ontologies struggle with generalization deficiencies.To address these challenges,this study proposes an OntologyAware LLM Methodology for Military Domain Knowledge Extraction(LLM-KE).This approach leverages the deep semantic comprehension capabilities of Large Language Models(LLMs)to simulate human experts’cognitive processes in crowdsourced ontology construction,enabling automated extraction of military textual knowledge.It concurrently enhances knowledge processing efficiency and improves KG completeness.Empirical analysis demonstrates that this method effectively resolves scalability and dynamic adaptation challenges in military KG construction,establishing a novel technological pathway for advancing military intelligence development.展开更多
AIM:To investigate the long-term outcomes in acute primary angle closure(APAC)patients treated with lens extraction(LE)surgery and to identify risk factors for glaucomatous optic neuropathy(GON).METHODS:In this longit...AIM:To investigate the long-term outcomes in acute primary angle closure(APAC)patients treated with lens extraction(LE)surgery and to identify risk factors for glaucomatous optic neuropathy(GON).METHODS:In this longitudinal observational study,detailed medical histories of APAC patients and comprehensive ophthalmic examinations at final followup were collected.Logistic regression analysis was performed to identify predictors of blindness.Univariate and multivariate linear regression analyses were conducted to determine risk factors associated with visual outcomes.RESULTS:This study included 39 affected eyes of 31 subjects(26 females)with an average age of 74.1±8.0y.At 6.7±4.2y after APAC attack,2(5.7%)eyes had bestcorrected visual acuity(VA)worse than 3/60.Advanced glaucomatous visual field loss was observed in 15(39.5%)affected eyes and 5(25.0%)fellow eyes.Nine affected eyes(23.7%)had GON,and 11(28.9%)were blind.Six(15.4%)affected eyes and 2(9.1%)fellow eyes had suspicious progression.A significantly higher blindness rate in factory workers compared to office workers.Logistic regression identified that worse VA at attack(OR 10.568,95%CI 1.288-86.695;P=0.028)and worse early postoperative VA(OR 13.214,95%CI 1.157-150.881;P=0.038)were risk factors for blindness.Multivariate regression showed that longer duration of elevated intraocular pressure(P=0.004)and worse early postoperative VA(P=0.009)were associated with worse visual outcomes.CONCLUSION:Despite LE surgery,some APAC patients experience continued visual function deterioration.Lifelong monitoring is necessary.Target pressure and progression rates should be re-evaluated during follow-up.展开更多
The physical properties and chemical components of three oil samples extracted from Illicium verum Hook. f. by steam distillation （SD）, solvent extraction （SE） and supercritical fluid extraction （SFE） were compa...The physical properties and chemical components of three oil samples extracted from Illicium verum Hook. f. by steam distillation （SD）, solvent extraction （SE） and supercritical fluid extraction （SFE） were compared with one another and analyzed by Gas Chromatography-Mass Spectrometry （GC-MS）. The quality parameters of star anise essential oil from SFE were close to that of those came from SD and SE. Although the extraction yield of star anise by SFE （9.2 %） was close to the value from SE （9.3%）, it was yet higher than that came from SD （8.2%）. For sensory evaluation, however, three oils were significantly different. The odor and taste of the products from SFE and SE were generally more natural and vivid than that came from distilled oil. The volatile compound revealed that significant differences of the composition existed in the distilled oil and the oleoresins prepared by SFE and SE.展开更多
Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol （OP） in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in su...Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol （OP） in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in surface water in Jinan, China was analyzed by gas chromatography-mass spectrometry （GC-MS） coupled with solid phase extraction （SPE）. Water samples were extracted by SPE on a cartridge system containing C-18 as sorbent. To increase sensitivity and selectivity, OP was derivatized to 4-tert-octyl-phenoxy silane. With the use of phenanthrene-d10 as internal standard, the detection limit based on signal-to-noise ratio （S/N = 3） was 0.06 ng/mL. The average recovery was from 84.67% to 109.7%. The precision of the method given as the relative standard deviations （RSD） was within the range 6.24%-12.96%. In the target water samples, the concentrations of OP were as follows： 15.88-71.24 ng/L for Jinxiuchuan Reservoir, 3.850-26.68 ng/L for the city moat, 6.930-41.56 ng/L for Daming Lake, 66.03-474.2 ng/L for Xiaoqing River, 14.66-17.72 ng/L for the Yellow River, and 10.60-26.43 ng/L for Queshan Reservoir. The Xiaoqing River was seriously polluted due to the discharge of wastewater from Jinan. Jinxiuchuan Reservoir had a higher concentration of OP compared with the Yellow River and Queshan Reservoir, which is ascribed to the surrounding human activities. These data are reported for the first time, providing strong support for the control of OP pollution in Jinan.展开更多
The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction （USE） and their chemical constituents were analyzed by gas chromatographymass spectrometry （GC-MS） to provide s...The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction （USE） and their chemical constituents were analyzed by gas chromatographymass spectrometry （GC-MS） to provide scientific basis for the quality control of safflower. Five different solvents （diethyl ether, ethanol, ethyl acetate, dichloromethane and acetone） were used and compared in terms of number of volatile components extracted and the peak areas of these components in TIC. The results showed that USE could be used as an efficient and rapid method for extracting the volatile components from safflower. It also could be found that the number of components in the TIC of ethyl acetate extract was more than that in the TIC of other solvent ones. Meanwhile, the volatile components of safflower from Xinjiang Autonomous Region and Henan Province of China were different in chemical components and relative contents. It could be concluded that both the extraction solvents and geographical origin of safflower are responsible for these differences. The experimental results also indicated that USE/GC-MS is a simple, rapid and effective method to analyze the volatile oil components of safflower.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
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
A rapid method was developed for the determination of 22 pesticides in rice wine. The procedure involved an extraction with acetonitrile and a cleanup step using dispersive solid-phase extraction (d-SPE), and primary-...A rapid method was developed for the determination of 22 pesticides in rice wine. The procedure involved an extraction with acetonitrile and a cleanup step using dispersive solid-phase extraction (d-SPE), and primary-secondary amine (PSA) and octadecylsilane (ODS) were used as sorbents. D-SPE had some advantages over some traditional prepara- tions, especially in time and cost. Both the extraction and cleanup only cost about 15 min per a sample. Then the GC-MS was used for quantitative and qualitative analysis. Matrix-matched standards solution and analyte protectant were compared to decrease the matrix effect, and the former showed a better efficacy. Acceptable linearity was achieved in the range of 0.05 - 0.30 mg/L. After matrix-matched standards calibration, recoveries were between 60 and 140%. For the most of pesticides, precision and repeatability were less than 10% and 16%, respectively. The result indicated that the developed method was suitable for the determination of the multi-pesticides in rice wine.展开更多
A modified analytical procedure has been developed to test for 5 organic pollutants [benzophenone, 2 diisopropylnaphthalenes (DIPNs) {2,6- and 2,7-diisopropylnapthalene} and 2 hydrogenated terphenyls (HTPs) {m-terphen...A modified analytical procedure has been developed to test for 5 organic pollutants [benzophenone, 2 diisopropylnaphthalenes (DIPNs) {2,6- and 2,7-diisopropylnapthalene} and 2 hydrogenated terphenyls (HTPs) {m-terphenyl and o-terphenyl}] that can be found as residues in recycled cardboards intended for use as food packaging materials and to test for migration levels of these compounds in a food simulant (Tenax). A main objective was to develop a modified rapid and reliable method for the identification and quantification of these compounds at low concentrations. The method was based on ultrasound-assisted solvent extraction (UAE) followed by gas chromatography-mass spectrometry (GC-MS) analysis. The developed method was applied to analyze 3 commercially available recycled carton board food-packaging materials and also to study the potential migration of the 5 organic pollutants from these materials into Tenax to check if these recycled cardboards can be considered as suitable for use in direct contact with foodstuffs. The limits of detection (LODs) of standard solutions of the 5 compounds were determined at a signal-to-noise ratio of 3. The LODs and the limits of quantification (LOQs) of examined pollutants ranged between 0.005 to 0.5 mg/kg, and 0.1 to 1 mg/kg, respectively. The extremely low amounts of most contaminants that migrate from packaging materials to Tenax indicate that the recycled cardboards tested can be safely used for direct food contact applications.展开更多
A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrumen...A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrument parameters including programmed oven temperature, injection temperature and ion source temperature were evaluated and optimized. Effects of extraction time, ionic strength and p H on the detection efficiency were investigated and optimum conditions were 8 min of extraction time, without Na Cl addition at p H=9. Good linearity(R2=0.9997) was obtained when the linear range was 10-500 μg/L. The recoveries of β-ionone in ultrapure water and tap water samples were 88%-95% and 110%-114%, respectively. The relative standard deviations(RSD) were less than 10%. The method detection limit(MDL) and rejection quality level(RQL) were achieved at1.98 μg/L and 6.53 μg/L, respectively. LLE-GC-MS was demonstrated to be a rapid and convenient method for the determination ofβ-ionone in water samples.展开更多
[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) com...[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.展开更多
本文通过以玉米碴为原料,酿酒酵母、嗜酸乳杆菌、枯草芽孢杆菌及纳豆芽孢杆菌作发酵剂,以单菌和组合的方式对玉米进行发酵制成玉米粉,采用气相-离子迁移谱(Gas-chromatography ion mobility spectrometry,GCIMS)和气相色谱-质谱联用(Gas...本文通过以玉米碴为原料,酿酒酵母、嗜酸乳杆菌、枯草芽孢杆菌及纳豆芽孢杆菌作发酵剂,以单菌和组合的方式对玉米进行发酵制成玉米粉,采用气相-离子迁移谱(Gas-chromatography ion mobility spectrometry,GCIMS)和气相色谱-质谱联用(Gas Chromatography-Mass Spectrometry,GC-MS)方法对发酵玉米粉的挥发性风味成分进行分析。结果表明,GC-IMS共检出68种风味物质,包括醛类12种、醇类18种、酯类11种、酮类11种以及6种杂环类;根据图谱差异分析发现,发酵后玉米粉风味物质均发生变化,其醇类、酯类和酸类物质含量相对提高。GC-MS共检出59种风味物质,包含13种醛类、12种酯类、15种醇类、7种酸类、6种酮类和7种杂环类物质。两种技术共同检测出29种风味物质,其中正癸醛等10种醛类、5种醇类、2-壬酮、2-庚酮、己酸乙酯、甲酸甲酯、丁酸乙酯及4种酸类物质为发酵玉米粉的主要风味物质。根据香气含量分析,对比未发酵玉米粉,自然发酵水果香含量提高了24.64%,酿酒酵母发酵水果香和酒香含量分别提高了30.05%、85.05%,嗜酸乳杆菌发酵水果甜香和奶油蜂蜜香含量分别提高了36.56%、90.36%,枯草芽孢杆菌和纳豆芽孢杆菌发酵水果甜香花及苦杏仁香含量分别提高了18.05%、15.59%和38.68%、38.02%,组合发酵水果甜香花、草香含量分别提高了53.53%、48.08%,表明经过发酵制得的玉米粉风味独特。展开更多
[Objective] This study aimed to analyze the chemical composition and yield of essential oil and n-hexane extract from moso bamboo to find active compounds with potential value. [Method] Essential oil and n-hexane extr...[Objective] This study aimed to analyze the chemical composition and yield of essential oil and n-hexane extract from moso bamboo to find active compounds with potential value. [Method] Essential oil and n-hexane extract were respectively extracted from moso bamboo of four different ages by using hydrodistillation and ultrasonic-assisted extraction with n-hexane, and analyzed with gas chromatography/mass spectrometry （GC/MS）. [Result] The results show that cedrol （46.39%） is the first principal volatile component in essential oil of the middle stem of 7-year old moso bamboo; dibutyl phthalate （59.46%） is the first principal volatile component in n-hexane extract of the middle stem of 3-year old moso bamboo; yield of n-hexane extract is higher than that of essential oil from moso bamboo. [Conclusion] Cedrol is an active compound with potential value.展开更多
基金supported by the National Natural Science Foundation of China(No.51939009)Shenzhen Science and Technology Program(Nos.JCYJ20241202125905008 and GXWD20201231165807007-20200810165349001).
文摘A trace analytical method based on solid-phase extraction gas chromatography-tandem mass spectrometry(SPE–GC–MS/MS)was developed for the rapid detection of 256 semi-volatile organic compounds(SVOCs),including 25 polycyclic aromatic hydrocarbons(PAHs),70 polychlorinated biphenyls(PCBs),123 pesticides,20 phthalate esters(PAEs),4 organophosphate esters(OPEs),9 synthetic musks(SMs),and 5 UV filters(UVs)in water.No-tably,this method provided a decent linearity of calibration standards(R^(2)>0.999),excellent method limits of quantification(MLOQs)(0.12–11.41 ng/L),satisfactory matrix spiking recovery rates(60.4%–126%),and high precision(intra-day relative standard deviations(RSDs):1.0%–10.0%,inter-day RSDs:3.0%–15.0%,and inter-week RSDs:3.4%–15.7%),making it suitable for trace-level studies.Statistical analysis revealed that SVOCs with higher volatility exhibited enhanced recovery rates.Validation of the methodology involved analyzing SVOCs in real spring water and river water samples.Twenty-seven SVOCs were detected in spring water and 58 in river water,with an average concentration of 631.73 and 16,095 ng/L,respectively.Among the detected SVOCs,PAEs constituted the predominant proportion.This study underscored the presence of SVOCs contamination specifi-cally within the spring water,although SVOCs concentrations in river water were significantly greater than those found in spring water.In summary,this sensitive method based on SPE–GC–MS/MS was successfully developed and validated for the rapid analysis of a diverse array of 256 SVOCs at trace levels in water,including not only the traditional highly valued PAHs,PCBs,pesticides,and PAEs,but also the emerging OPEs,UVs,and SMs.
基金Supported by Undergraduate Innovation Training Program of Jiangsu Province(201610327010Z)~~
文摘[Objective] This study was aimed to determine the optimal parameters for the extraction of perilla seed oil to obtain high-quality perilla seed oil and analyze its compositions. [Method] In this study, perilla seed oil was extracted using supercritical CO2 （SC-CO2）. The effects of extraction time, temperature and pressure were investigated by single-factor experiments and orthogonal array testing （ORT）. The chemical compositions of extracted perilla seed oil were investigated by GC-MS. [Result] The optimal conditions for the extraction of perilla seed oil using SC-CO2 were extraction time of 4 h, extraction temperature at 40 ℃, and extraction pressure at 23 MPa. Under these conditions, the extraction yield of perilla seed oil was maximized to 12.43%. GC-MS analysis revealed that perilla seed oil was a complex mixture containing 76.183% α-linolenic acid. [Conclusion] Supercritical CO2 extraction was proven to be an effective technology to extract oil from perilla seed, and GCMS was also a satisfactory method for analyzing the compositions of perilla seed oil.
文摘To determine the chemical constituents of volatile components in saffron from the Tibet Autonomous Region and the Henan Province of China and to compare the chemical composition difference in the saffron,the total volatile components were extracted by ultrasonic-assisted solvent extraction（USE）,using five different solvents：diethyl ether,ethanol,ethyl acetate, dichloromethane and acetone,analyzed using gas chromatography-mass spectrometry（GC-MS）and compared to the standard MS data,and their relative contents were calculated by area normalization.The results showed both that USE was an efficient and rapid method for the extraction of the volatile components from saffron and that the components extracted from the same sample using different solvents were different.Comparison of the experimental results of saffron from the Tibet Autonomous Region and the Henan Province of China showed that their volatile components were different in their chemical composition and in their relative percentages.USE/GC-MS is a simple,rapid,and effective method for the analysis of volatile oil components in saffron.
基金supported by the National Natural Science Foundation of China(No.82204610)Qihang Talent Program(L2022046)+1 种基金the Scientific and Technological Innovation Project of China Academy of Chinese Medical Sciences(CI2021A04013)Fundamental Research Funds for the Central Public Welfare Research Institutes(ZZ15-YQ-041 and L2021029).
文摘Background:Cyperi Rhizoma,derived from Cyperus rotundus L.,is a widely used medicinal herb in traditional Chinese medicine(TCM),with Shandong Province recognized as its geo-authentic habitat.However,the quality of Cyperi Rhizoma varies significantly across different regions,potentially influencing its therapeutic efficacy.This study investigates the influence of geographic origin on the chemical composition and overall quality of Cyperi Rhizoma.Methods:A comprehensive approach,including traditional quality assessment,GC-MS(g as c hromatography-m ass s pectrometry),RP-HPLC(r everse p hase h igh-p erformance l iquid c hromatography),and FT-IR(f ourier t ransform i nfrared s pectroscopy)techniques,was employed to analyze Cyperi Rhizoma samples from Shandong Province.These methods examined the physical appearance,chemical profile,and content variations,particularly focusing onα-cyperone.Results:Traditional quality assessments revealed noticeable differences in the external characteristics of the samples.GC-MS analysis identified a variety of unique chemical constituents,while RP-HPLC and FT-IR showed significant variations inα-cyperone content,with higher levels found in Shandong samples.Conclusion:These results demonstrate that geographic origin is a critical determinant of Cyperi Rhizoma quality,with Shandong specimens exhibiting superiorα-cyperone levels and characteristic phytochemical profiles.This validates the geo-authenticity concept in TCM and provides actionable data for developing evidence-based quality standards,suggesting that provenance should be prioritized in medicinal material selection and pharmacopeial specifications.
文摘Since Google introduced the concept of Knowledge Graphs(KGs)in 2012,their construction technologies have evolved into a comprehensive methodological framework encompassing knowledge acquisition,extraction,representation,modeling,fusion,computation,and storage.Within this framework,knowledge extraction,as the core component,directly determines KG quality.In military domains,traditional manual curation models face efficiency constraints due to data fragmentation,complex knowledge architectures,and confidentiality protocols.Meanwhile,crowdsourced ontology construction approaches from general domains prove non-transferable,while human-crafted ontologies struggle with generalization deficiencies.To address these challenges,this study proposes an OntologyAware LLM Methodology for Military Domain Knowledge Extraction(LLM-KE).This approach leverages the deep semantic comprehension capabilities of Large Language Models(LLMs)to simulate human experts’cognitive processes in crowdsourced ontology construction,enabling automated extraction of military textual knowledge.It concurrently enhances knowledge processing efficiency and improves KG completeness.Empirical analysis demonstrates that this method effectively resolves scalability and dynamic adaptation challenges in military KG construction,establishing a novel technological pathway for advancing military intelligence development.
文摘AIM:To investigate the long-term outcomes in acute primary angle closure(APAC)patients treated with lens extraction(LE)surgery and to identify risk factors for glaucomatous optic neuropathy(GON).METHODS:In this longitudinal observational study,detailed medical histories of APAC patients and comprehensive ophthalmic examinations at final followup were collected.Logistic regression analysis was performed to identify predictors of blindness.Univariate and multivariate linear regression analyses were conducted to determine risk factors associated with visual outcomes.RESULTS:This study included 39 affected eyes of 31 subjects(26 females)with an average age of 74.1±8.0y.At 6.7±4.2y after APAC attack,2(5.7%)eyes had bestcorrected visual acuity(VA)worse than 3/60.Advanced glaucomatous visual field loss was observed in 15(39.5%)affected eyes and 5(25.0%)fellow eyes.Nine affected eyes(23.7%)had GON,and 11(28.9%)were blind.Six(15.4%)affected eyes and 2(9.1%)fellow eyes had suspicious progression.A significantly higher blindness rate in factory workers compared to office workers.Logistic regression identified that worse VA at attack(OR 10.568,95%CI 1.288-86.695;P=0.028)and worse early postoperative VA(OR 13.214,95%CI 1.157-150.881;P=0.038)were risk factors for blindness.Multivariate regression showed that longer duration of elevated intraocular pressure(P=0.004)and worse early postoperative VA(P=0.009)were associated with worse visual outcomes.CONCLUSION:Despite LE surgery,some APAC patients experience continued visual function deterioration.Lifelong monitoring is necessary.Target pressure and progression rates should be re-evaluated during follow-up.
基金Supported by the Science and Technology Key Project of Guangxi Province (0424008-1C)
文摘The physical properties and chemical components of three oil samples extracted from Illicium verum Hook. f. by steam distillation （SD）, solvent extraction （SE） and supercritical fluid extraction （SFE） were compared with one another and analyzed by Gas Chromatography-Mass Spectrometry （GC-MS）. The quality parameters of star anise essential oil from SFE were close to that of those came from SD and SE. Although the extraction yield of star anise by SFE （9.2 %） was close to the value from SE （9.3%）, it was yet higher than that came from SD （8.2%）. For sensory evaluation, however, three oils were significantly different. The odor and taste of the products from SFE and SE were generally more natural and vivid than that came from distilled oil. The volatile compound revealed that significant differences of the composition existed in the distilled oil and the oleoresins prepared by SFE and SE.
基金supported by the State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences (No. KF2009-13)the National Natural Science Foundation of China (No. 21007019, 21107030,21277059, 21277060)
文摘Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol （OP） in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in surface water in Jinan, China was analyzed by gas chromatography-mass spectrometry （GC-MS） coupled with solid phase extraction （SPE）. Water samples were extracted by SPE on a cartridge system containing C-18 as sorbent. To increase sensitivity and selectivity, OP was derivatized to 4-tert-octyl-phenoxy silane. With the use of phenanthrene-d10 as internal standard, the detection limit based on signal-to-noise ratio （S/N = 3） was 0.06 ng/mL. The average recovery was from 84.67% to 109.7%. The precision of the method given as the relative standard deviations （RSD） was within the range 6.24%-12.96%. In the target water samples, the concentrations of OP were as follows： 15.88-71.24 ng/L for Jinxiuchuan Reservoir, 3.850-26.68 ng/L for the city moat, 6.930-41.56 ng/L for Daming Lake, 66.03-474.2 ng/L for Xiaoqing River, 14.66-17.72 ng/L for the Yellow River, and 10.60-26.43 ng/L for Queshan Reservoir. The Xiaoqing River was seriously polluted due to the discharge of wastewater from Jinan. Jinxiuchuan Reservoir had a higher concentration of OP compared with the Yellow River and Queshan Reservoir, which is ascribed to the surrounding human activities. These data are reported for the first time, providing strong support for the control of OP pollution in Jinan.
文摘The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction （USE） and their chemical constituents were analyzed by gas chromatographymass spectrometry （GC-MS） to provide scientific basis for the quality control of safflower. Five different solvents （diethyl ether, ethanol, ethyl acetate, dichloromethane and acetone） were used and compared in terms of number of volatile components extracted and the peak areas of these components in TIC. The results showed that USE could be used as an efficient and rapid method for extracting the volatile components from safflower. It also could be found that the number of components in the TIC of ethyl acetate extract was more than that in the TIC of other solvent ones. Meanwhile, the volatile components of safflower from Xinjiang Autonomous Region and Henan Province of China were different in chemical components and relative contents. It could be concluded that both the extraction solvents and geographical origin of safflower are responsible for these differences. The experimental results also indicated that USE/GC-MS is a simple, rapid and effective method to analyze the volatile oil components of safflower.
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 (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.
文摘A rapid method was developed for the determination of 22 pesticides in rice wine. The procedure involved an extraction with acetonitrile and a cleanup step using dispersive solid-phase extraction (d-SPE), and primary-secondary amine (PSA) and octadecylsilane (ODS) were used as sorbents. D-SPE had some advantages over some traditional prepara- tions, especially in time and cost. Both the extraction and cleanup only cost about 15 min per a sample. Then the GC-MS was used for quantitative and qualitative analysis. Matrix-matched standards solution and analyte protectant were compared to decrease the matrix effect, and the former showed a better efficacy. Acceptable linearity was achieved in the range of 0.05 - 0.30 mg/L. After matrix-matched standards calibration, recoveries were between 60 and 140%. For the most of pesticides, precision and repeatability were less than 10% and 16%, respectively. The result indicated that the developed method was suitable for the determination of the multi-pesticides in rice wine.
文摘A modified analytical procedure has been developed to test for 5 organic pollutants [benzophenone, 2 diisopropylnaphthalenes (DIPNs) {2,6- and 2,7-diisopropylnapthalene} and 2 hydrogenated terphenyls (HTPs) {m-terphenyl and o-terphenyl}] that can be found as residues in recycled cardboards intended for use as food packaging materials and to test for migration levels of these compounds in a food simulant (Tenax). A main objective was to develop a modified rapid and reliable method for the identification and quantification of these compounds at low concentrations. The method was based on ultrasound-assisted solvent extraction (UAE) followed by gas chromatography-mass spectrometry (GC-MS) analysis. The developed method was applied to analyze 3 commercially available recycled carton board food-packaging materials and also to study the potential migration of the 5 organic pollutants from these materials into Tenax to check if these recycled cardboards can be considered as suitable for use in direct contact with foodstuffs. The limits of detection (LODs) of standard solutions of the 5 compounds were determined at a signal-to-noise ratio of 3. The LODs and the limits of quantification (LOQs) of examined pollutants ranged between 0.005 to 0.5 mg/kg, and 0.1 to 1 mg/kg, respectively. The extremely low amounts of most contaminants that migrate from packaging materials to Tenax indicate that the recycled cardboards tested can be safely used for direct food contact applications.
基金Project(51178321)supported by the National Natural Science Foundation of ChinaProject(2012ZX07403-001)supported by the National Science and Technology Major Project,ChinaProject(20120072110050)supported by the Research Fund for the Doctoral Program of Higher Education of China
文摘A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrument parameters including programmed oven temperature, injection temperature and ion source temperature were evaluated and optimized. Effects of extraction time, ionic strength and p H on the detection efficiency were investigated and optimum conditions were 8 min of extraction time, without Na Cl addition at p H=9. Good linearity(R2=0.9997) was obtained when the linear range was 10-500 μg/L. The recoveries of β-ionone in ultrapure water and tap water samples were 88%-95% and 110%-114%, respectively. The relative standard deviations(RSD) were less than 10%. The method detection limit(MDL) and rejection quality level(RQL) were achieved at1.98 μg/L and 6.53 μg/L, respectively. LLE-GC-MS was demonstrated to be a rapid and convenient method for the determination ofβ-ionone in water samples.
基金Supported by Key Science and Technology Project of Gansu Province(1302NKDA028)Science and Technology Planning Project of Lanzhou(2010-1-239+2 种基金 2016-3-4)Talent Project of Lanzhou Science and Technology Bureau(2015-RC-87)Project of Science and Technology Cooperation between Gansu Academy of Agricultural Sciences and Local Areas(2017GAAS63)
文摘[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.
基金Supported by Sub-project of the "Eleventh Five-Year" National Science and Technology Support Program (2006BAD19B04)~~
文摘[Objective] This study aimed to analyze the chemical composition and yield of essential oil and n-hexane extract from moso bamboo to find active compounds with potential value. [Method] Essential oil and n-hexane extract were respectively extracted from moso bamboo of four different ages by using hydrodistillation and ultrasonic-assisted extraction with n-hexane, and analyzed with gas chromatography/mass spectrometry （GC/MS）. [Result] The results show that cedrol （46.39%） is the first principal volatile component in essential oil of the middle stem of 7-year old moso bamboo; dibutyl phthalate （59.46%） is the first principal volatile component in n-hexane extract of the middle stem of 3-year old moso bamboo; yield of n-hexane extract is higher than that of essential oil from moso bamboo. [Conclusion] Cedrol is an active compound with potential value.
