The volatile compounds emitted from Mosla chinensis Maxim were analyzed by headspace solid-phase micro- extraction （HS-SPME） and headspace liquid-phase microextraction （HS-LPME） combined with gas chromatography-ma...The volatile compounds emitted from Mosla chinensis Maxim were analyzed by headspace solid-phase micro- extraction （HS-SPME） and headspace liquid-phase microextraction （HS-LPME） combined with gas chromatography-mass spectrometry （GC-MS）. The main volatiles from Mosla chinensis Maxim were studied in this paper. It can be seen that 61 compounds were separated and identified. Forty-nine volatile compounds were identified by SPME method, mainly including myrcene, a-terpinene, p-cymene, （E）-ocimene, thymol, thymol acetate and （E）-fl-farnesene. Forty-five major volatile compounds were identified by LPME method, including a-thujene, a-pinene, camphene, butanoic acid, 2-methylpropyl ester, myrcene, butanoic acid, butyl ester, a-terpinene, p-cymene, （E）-ocimene, butane, 1,1-dibutoxy-, thymol, thymol acetate and （E）-fl-farnesene. After analyzing the volatile compounds, multiple linear regression （MLR） method was used for building the regression model. Then the quantitative structure-retention relationship （QSRR） model was validated by predictive-ability test. The prediction results were in good agreement with the experimental values. The results demonstrated that headspace SPME-GC-MS and LPME-GC-MS are the simple, rapid and easy sample enrichment technique suitable for analysis of volatile compounds. This investigation provided an effective method for predicting the retention indices of new compounds even in the absence of the standard candidates.展开更多
Determination methods of trace Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) were established based on the combination of LPME of dithizone-chelate for high enrichment,strip shape sampling-TLC and digital image-processing for quantitative...Determination methods of trace Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) were established based on the combination of LPME of dithizone-chelate for high enrichment,strip shape sampling-TLC and digital image-processing for quantitative analysis.Detection limits of Cu(Ⅱ),Hg(Ⅱ) and Cd(Ⅱ) were 1.5 ng/mL,1.3 ng/mL and 2.5ng/mL,respectively.RSDs were 1.2%,4.0% and 2.7%,respectively.The proposed methods have the advantages of convenience,sensitiveness,precise and economicls.The methods were applied to the determination of these elements in a pool water and mud,with satisfying results.展开更多
A two-phase hollow-fiber (HF) liquid-phase microextraction (LPME) method followed by gas chromatography was developed for quantification of 8 major polybrominated diphenyl ethers at trace level in sewage sludge. In th...A two-phase hollow-fiber (HF) liquid-phase microextraction (LPME) method followed by gas chromatography was developed for quantification of 8 major polybrominated diphenyl ethers at trace level in sewage sludge. In this method the porous polypropylene hollow fibers filled with a few microliters of organic solvent, were immersed in aqueous samples of wet sludge which were spiked with the PBDEs at ng/l level. Parameters such as salt concentration, stirring speed, extraction time and pH were optimized and the optimum extraction conditions were then applied to the determination of PBDEs in sewage sludge from K?llby sewage treatment plant in Lund. The optimized method allowed detection of 5.1 μg kg–1 and 0.43 μg kg–1 of BDE-47 and 183, respectively, in dried sludge. The findings were compatible with the results from recent research on PBDEs level in sewage sludge samples from Sweden. Although BDE-209 was expected to have the highest level, it was not detected. Limit of detection, photodegradation or/and biodegradation of BDE-209 during treatment or experiment are major reasons. Low organic solvent consumption, low sample volume requirement, high preconcentration factor, simplicity without using expensive instrument for extraction and excellent sample clean-up are some important factors that make this sample preparation technique very useful for determination of PBDEs in sludge.展开更多
建立了顶空液相微萃取/气相色谱-质谱联用测定中药枳壳中有机挥发物的方法。在顶空液相微萃取实验条件优化的基础上,确定了最佳实验条件:以正辛烷作为有机萃取剂,体积为2μL,样品用量为0.3g,液滴距离样品表面0.8 cm处,萃取8 m in后直接...建立了顶空液相微萃取/气相色谱-质谱联用测定中药枳壳中有机挥发物的方法。在顶空液相微萃取实验条件优化的基础上,确定了最佳实验条件:以正辛烷作为有机萃取剂,体积为2μL,样品用量为0.3g,液滴距离样品表面0.8 cm处,萃取8 m in后直接进样。与固相微萃取/气相色谱-质谱法相比,顶空液相微萃取法定性了30种成分,固相微萃取法定性了24种成分,顶空液相微萃取法操作简单、快速,实验结果灵敏度更高,且萃取效率高,重复性好,可用于中药枳壳中有机挥发物的快速分析。展开更多
基金Project supported by the Natural Science Foundation Programof Zhejiang Province （No. Y407308）, the Ministry of Science and Technology of Zhejiang Province （No. 201 OR 10044） and the Sprout Talented Project Program of Zhejiang Province （No. 2008R40G2020019）.
文摘The volatile compounds emitted from Mosla chinensis Maxim were analyzed by headspace solid-phase micro- extraction （HS-SPME） and headspace liquid-phase microextraction （HS-LPME） combined with gas chromatography-mass spectrometry （GC-MS）. The main volatiles from Mosla chinensis Maxim were studied in this paper. It can be seen that 61 compounds were separated and identified. Forty-nine volatile compounds were identified by SPME method, mainly including myrcene, a-terpinene, p-cymene, （E）-ocimene, thymol, thymol acetate and （E）-fl-farnesene. Forty-five major volatile compounds were identified by LPME method, including a-thujene, a-pinene, camphene, butanoic acid, 2-methylpropyl ester, myrcene, butanoic acid, butyl ester, a-terpinene, p-cymene, （E）-ocimene, butane, 1,1-dibutoxy-, thymol, thymol acetate and （E）-fl-farnesene. After analyzing the volatile compounds, multiple linear regression （MLR） method was used for building the regression model. Then the quantitative structure-retention relationship （QSRR） model was validated by predictive-ability test. The prediction results were in good agreement with the experimental values. The results demonstrated that headspace SPME-GC-MS and LPME-GC-MS are the simple, rapid and easy sample enrichment technique suitable for analysis of volatile compounds. This investigation provided an effective method for predicting the retention indices of new compounds even in the absence of the standard candidates.
文摘Determination methods of trace Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) were established based on the combination of LPME of dithizone-chelate for high enrichment,strip shape sampling-TLC and digital image-processing for quantitative analysis.Detection limits of Cu(Ⅱ),Hg(Ⅱ) and Cd(Ⅱ) were 1.5 ng/mL,1.3 ng/mL and 2.5ng/mL,respectively.RSDs were 1.2%,4.0% and 2.7%,respectively.The proposed methods have the advantages of convenience,sensitiveness,precise and economicls.The methods were applied to the determination of these elements in a pool water and mud,with satisfying results.
文摘A two-phase hollow-fiber (HF) liquid-phase microextraction (LPME) method followed by gas chromatography was developed for quantification of 8 major polybrominated diphenyl ethers at trace level in sewage sludge. In this method the porous polypropylene hollow fibers filled with a few microliters of organic solvent, were immersed in aqueous samples of wet sludge which were spiked with the PBDEs at ng/l level. Parameters such as salt concentration, stirring speed, extraction time and pH were optimized and the optimum extraction conditions were then applied to the determination of PBDEs in sewage sludge from K?llby sewage treatment plant in Lund. The optimized method allowed detection of 5.1 μg kg–1 and 0.43 μg kg–1 of BDE-47 and 183, respectively, in dried sludge. The findings were compatible with the results from recent research on PBDEs level in sewage sludge samples from Sweden. Although BDE-209 was expected to have the highest level, it was not detected. Limit of detection, photodegradation or/and biodegradation of BDE-209 during treatment or experiment are major reasons. Low organic solvent consumption, low sample volume requirement, high preconcentration factor, simplicity without using expensive instrument for extraction and excellent sample clean-up are some important factors that make this sample preparation technique very useful for determination of PBDEs in sludge.
文摘建立了顶空液相微萃取/气相色谱-质谱联用测定中药枳壳中有机挥发物的方法。在顶空液相微萃取实验条件优化的基础上,确定了最佳实验条件:以正辛烷作为有机萃取剂,体积为2μL,样品用量为0.3g,液滴距离样品表面0.8 cm处,萃取8 m in后直接进样。与固相微萃取/气相色谱-质谱法相比,顶空液相微萃取法定性了30种成分,固相微萃取法定性了24种成分,顶空液相微萃取法操作简单、快速,实验结果灵敏度更高,且萃取效率高,重复性好,可用于中药枳壳中有机挥发物的快速分析。
