The volatile and semi-volatile components in tobacco flavor additives were extracted by both simultaneous distillation extraction and solid-phase micro-extraction. Extraction conditions for solid-phase micro-extractio...The volatile and semi-volatile components in tobacco flavor additives were extracted by both simultaneous distillation extraction and solid-phase micro-extraction. Extraction conditions for solid-phase micro-extraction were optimized with information theory. Then, detection were accomplished by gas chromatography-mass spectrometry. Characteristic of each method was compared. Qualitative analysis and quantitative analysis of 6# tobacco flavor sample were accomplished through both simultaneous distillation extraction and solid-phase micro-extraction. The experimental results show that solid-phase micro-extraction method is the first choice for qualitative analysis and simultaneous distillation extraction is another good selection for quantitative analysis. By means of simultaneous distillation extraction, 20 components are identified, accounting for 92.77% of the total peak areas. Through solid-phase micro-extraction, there are 17 components identified accounting for 91.49% of the total peak areas. The main aromatic components in 6# tobacco flavor sample are propanoic acid, 2-hydroxy-, ethyl ester, menthol and menthyl acetate. The presented method has been successfully used for quality control of tobacco flavor.展开更多
A rapid headspace single-drop micro-extraction（mix） gas chromatography mass spectrometry（SDMEGC -MS） for the analysis of the volatile compounds in Herba Asari was developed in this study.A mixed solvent of n-tride...A rapid headspace single-drop micro-extraction（mix） gas chromatography mass spectrometry（SDMEGC -MS） for the analysis of the volatile compounds in Herba Asari was developed in this study.A mixed solvent of n-tridecane and butyl acetate（1：1） was finally used for the extraction at 70 C for 15 min with sample amount of 0.750 g and 100 mesh particle size.Under the determined conditions,the pound samples of Herba Asari were directly applied for the analysis.SDME-GC-MS,SPME-GC-MS and SD-GCMS methods were compared and the results showed that SDME-GC-MS method was a simple, inexpensive and effective way to measure the volatile compounds in Herba Asari and could be used for the analysis of volatile compounds in complex samples.展开更多
Solid phase extraction （SPE） is a widely used sample pretreatment method for separation, purification and enrichment, which has been established due to its significant advantages of time-saving, low consumption of s...Solid phase extraction （SPE） is a widely used sample pretreatment method for separation, purification and enrichment, which has been established due to its significant advantages of time-saving, low consumption of solvent, high enrichment factor, high accuracy, etc. In recent years, a variety of new SPE methods such as molecularly imprinted solid phase extraction （MISPE）, magnetic solid phase extraction （MSPE）, solid phase micro-extraction （SPME）, etc., which are superior to the conventional SPE, have been developed and been widely applied to food, drugs, and environmental monitoring. In this paper, the basic principles and methods of SPE and its new applications in different areas are reviewed.展开更多
Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sam...Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sample processing. To meet these emerging demands on biopharmaceutical analysis, this paper summarizes several new techniques of on-line biological sample processing: solid phase extraction, solid phase micro-extraction, column switching, limited intake filler, molecularly imprinted solid phase extraction, tubular column, and micro-dialysis. We describe new developments, principles, and characteristics of these techniques, and the application of liquid chromatography mass spectrometry (LC MS) in biopharmaceutical analysis with these new techniques in on-line biological sample processing. (C) 2016 Chinese Pharmaceutical Association and Institute of Materia Medica, Chinese Academy of Medical Sciences. Production and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND展开更多
Quality control of ginseng currently is mainly based on ginsenoside analysis,but rarely focuses on the volatile organic components.In the current work,an untargeted metabolomics approach,by headspace solid-phase micro...Quality control of ginseng currently is mainly based on ginsenoside analysis,but rarely focuses on the volatile organic components.In the current work,an untargeted metabolomics approach,by headspace solid-phase micro-extraction gas chromatography/mass spectrometry(HS-SPME-GC/MS),was elaborated and further employed to holistically compare the compositional difference of the volatile components simultaneously from 12 Panax herbal medicines,which included P.ginseng(PG),P.quinquefolius(PQ),P.notoginseng(PN),red ginseng(PGR),P.ginseng leaf(PGL),P.quinquefolius leaf(PQL),P.notoginseng leaf(PNL),P.ginseng flower(PGF),P.quinquefolius flower(PQF),P.notoginseng flower(PNF),P.japonicus(PJ),and P.japonicus var.major(PJvm).Chromatographic separation was performed on an HP-5MS elastic quartz capillary column using helium as the carrier gas,enabling good resolution within 1 h.We were able to characterize totally 259 volatile compounds,including 82 terpenes(T),46 alcohols(Alc),29 ketones(K),25 aldehydes(Ald),21 esters(E),and the others.By analyzing 90 batches of ginseng samples based on the untargeted metabolomics workflows,236 differential ions were unveiled,and accordingly 36 differential volatile components were discovered.It is the first report that simultaneously compares the compositional difference of volatile components among 12 Panax herbal medicines,and useful information is provided for the quality control of ginseng aside from the well-known ginsenosides.展开更多
[Objective] To analyze the volatile flavor compounds in mutton of different parts of Ningxia Tan sheep. [Method] The volatile flavor compounds in mutton were identified and quantified using the solid phase micro-extra...[Objective] To analyze the volatile flavor compounds in mutton of different parts of Ningxia Tan sheep. [Method] The volatile flavor compounds in mutton were identified and quantified using the solid phase micro-extraction （SPME） method combined with GC-MS analysis. [ Re- sult ] The proportion of aldehydes in volatile compounds was the highest in the mutton of most parts of Ningxia Tan sheep, but no 4-methyl acid and 4-methyl nonyl acid was detected in the mutton. [ Conclusion]Aldehydes may be important for the volatile flavor of mutton of Ningxia Tan sheep. The study provides a basis for better development and use of Ningxia Tan sheep.展开更多
A method for rapid identification and quantification of phthalate plasticizers in beverages was developed.A number of 15 phthalate plasticizers which covered all the phthalates concerned in the US Consumer Product Saf...A method for rapid identification and quantification of phthalate plasticizers in beverages was developed.A number of 15 phthalate plasticizers which covered all the phthalates concerned in the US Consumer Product Safety Improvement Act(CPSIA),European Union legislations and Chinese national standards(GB)were analyzed.By a combined solid-phase micro-extraction(SPME)and direct analysis in real time mass spectrometry(DART-MS)approach,phthalates at sub-ng•mL^(−1)levels can be qualitatively and quantitatively analyzed in a short time.The use of ultrahigh-resolving power and the accurate mass measurement capacity naturally provided by Fourier transform ion cyclotron resonance mass spectrometry(FT-ICR-MS)minimizes the matrix interferences and thus enables the evaluation of phthalates in a complex matrix without extensive sample handlings or preparations.The limits of quantification(LOQs)were estimated to be at 0.3-5.0 ng•mL^(−1),lower than the Maximum Residue Limit(MRL)regulated by the European Union legislations(2007/19/EC)in foods,beverages,food packaging and toys(0.3-30 ng•mL^(−1)).This rapid and easy-to-use SPME-DART-FT-ICR-MS method provided a relatively high-throughput and powerful analytical approach for quick testing and screening phthalates in beverages and water samples to ensure food safety.展开更多
An analytical method using gas chromatography isotope ratio mass spectrometry(GC-IRMS)combined with solid phase micro-extraction(SPME)was developed to measure the 613C values of six typical volatiles commonly occurrin...An analytical method using gas chromatography isotope ratio mass spectrometry(GC-IRMS)combined with solid phase micro-extraction(SPME)was developed to measure the 613C values of six typical volatiles commonly occurring in wine(isoamyl acetate,2-octanone,limonene,2-phenylethanol,ethyl octanoate and ethyl decanoate)for the first time.SPME selected with a divinylbenzene/carboxen/polydimethylsiloxane fiber was combined with the GC-IRMS for pretreatment optimization.The optimized SPME parameters of extraction time,extraction temperature and salt concentration were 40 min,40℃ and 10%,respectively.The 613C values measured by SPME-GC-IRMS were in good agreement with those measured via elemental analyzer(EA)-IRMS and GC-IRMS.The differences range from 0.02‰to 0.44‰ with EA-IRMS and from 0 to 0.28‰ with GC-IRMS,indicating the high accuracy of the method.This newly established method measured the precision within 0.30‰ and was successfully validated to discriminate imported real wine samples with identical label but amazing price differences from different importers.展开更多
文摘The volatile and semi-volatile components in tobacco flavor additives were extracted by both simultaneous distillation extraction and solid-phase micro-extraction. Extraction conditions for solid-phase micro-extraction were optimized with information theory. Then, detection were accomplished by gas chromatography-mass spectrometry. Characteristic of each method was compared. Qualitative analysis and quantitative analysis of 6# tobacco flavor sample were accomplished through both simultaneous distillation extraction and solid-phase micro-extraction. The experimental results show that solid-phase micro-extraction method is the first choice for qualitative analysis and simultaneous distillation extraction is another good selection for quantitative analysis. By means of simultaneous distillation extraction, 20 components are identified, accounting for 92.77% of the total peak areas. Through solid-phase micro-extraction, there are 17 components identified accounting for 91.49% of the total peak areas. The main aromatic components in 6# tobacco flavor sample are propanoic acid, 2-hydroxy-, ethyl ester, menthol and menthyl acetate. The presented method has been successfully used for quality control of tobacco flavor.
文摘A rapid headspace single-drop micro-extraction（mix） gas chromatography mass spectrometry（SDMEGC -MS） for the analysis of the volatile compounds in Herba Asari was developed in this study.A mixed solvent of n-tridecane and butyl acetate（1：1） was finally used for the extraction at 70 C for 15 min with sample amount of 0.750 g and 100 mesh particle size.Under the determined conditions,the pound samples of Herba Asari were directly applied for the analysis.SDME-GC-MS,SPME-GC-MS and SD-GCMS methods were compared and the results showed that SDME-GC-MS method was a simple, inexpensive and effective way to measure the volatile compounds in Herba Asari and could be used for the analysis of volatile compounds in complex samples.
基金supported by the Key Laboratory for Rare Disease of Shandong Province
文摘Solid phase extraction （SPE） is a widely used sample pretreatment method for separation, purification and enrichment, which has been established due to its significant advantages of time-saving, low consumption of solvent, high enrichment factor, high accuracy, etc. In recent years, a variety of new SPE methods such as molecularly imprinted solid phase extraction （MISPE）, magnetic solid phase extraction （MSPE）, solid phase micro-extraction （SPME）, etc., which are superior to the conventional SPE, have been developed and been widely applied to food, drugs, and environmental monitoring. In this paper, the basic principles and methods of SPE and its new applications in different areas are reviewed.
基金supported by the National Natural Science Foundation of China(No.81102499)the Fundamental Research Funds for the Central Universities of Central South University and Hunan Science and Technology Project(No.2011SK3261)
文摘Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sample processing. To meet these emerging demands on biopharmaceutical analysis, this paper summarizes several new techniques of on-line biological sample processing: solid phase extraction, solid phase micro-extraction, column switching, limited intake filler, molecularly imprinted solid phase extraction, tubular column, and micro-dialysis. We describe new developments, principles, and characteristics of these techniques, and the application of liquid chromatography mass spectrometry (LC MS) in biopharmaceutical analysis with these new techniques in on-line biological sample processing. (C) 2016 Chinese Pharmaceutical Association and Institute of Materia Medica, Chinese Academy of Medical Sciences. Production and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND
基金National Natural Science Foundation of China(Grant No.81872996)Natural Science Foundation of Tianjin of China(Grant No.20JCYBJC00060).
文摘Quality control of ginseng currently is mainly based on ginsenoside analysis,but rarely focuses on the volatile organic components.In the current work,an untargeted metabolomics approach,by headspace solid-phase micro-extraction gas chromatography/mass spectrometry(HS-SPME-GC/MS),was elaborated and further employed to holistically compare the compositional difference of the volatile components simultaneously from 12 Panax herbal medicines,which included P.ginseng(PG),P.quinquefolius(PQ),P.notoginseng(PN),red ginseng(PGR),P.ginseng leaf(PGL),P.quinquefolius leaf(PQL),P.notoginseng leaf(PNL),P.ginseng flower(PGF),P.quinquefolius flower(PQF),P.notoginseng flower(PNF),P.japonicus(PJ),and P.japonicus var.major(PJvm).Chromatographic separation was performed on an HP-5MS elastic quartz capillary column using helium as the carrier gas,enabling good resolution within 1 h.We were able to characterize totally 259 volatile compounds,including 82 terpenes(T),46 alcohols(Alc),29 ketones(K),25 aldehydes(Ald),21 esters(E),and the others.By analyzing 90 batches of ginseng samples based on the untargeted metabolomics workflows,236 differential ions were unveiled,and accordingly 36 differential volatile components were discovered.It is the first report that simultaneously compares the compositional difference of volatile components among 12 Panax herbal medicines,and useful information is provided for the quality control of ginseng aside from the well-known ginsenosides.
基金funded by the Key Technology R&D Program of Ningxia Hui Autonomous Region
文摘[Objective] To analyze the volatile flavor compounds in mutton of different parts of Ningxia Tan sheep. [Method] The volatile flavor compounds in mutton were identified and quantified using the solid phase micro-extraction （SPME） method combined with GC-MS analysis. [ Re- sult ] The proportion of aldehydes in volatile compounds was the highest in the mutton of most parts of Ningxia Tan sheep, but no 4-methyl acid and 4-methyl nonyl acid was detected in the mutton. [ Conclusion]Aldehydes may be important for the volatile flavor of mutton of Ningxia Tan sheep. The study provides a basis for better development and use of Ningxia Tan sheep.
基金support from National Natural Science Foundation of China(Nos.21172250 and 21275155).
文摘A method for rapid identification and quantification of phthalate plasticizers in beverages was developed.A number of 15 phthalate plasticizers which covered all the phthalates concerned in the US Consumer Product Safety Improvement Act(CPSIA),European Union legislations and Chinese national standards(GB)were analyzed.By a combined solid-phase micro-extraction(SPME)and direct analysis in real time mass spectrometry(DART-MS)approach,phthalates at sub-ng•mL^(−1)levels can be qualitatively and quantitatively analyzed in a short time.The use of ultrahigh-resolving power and the accurate mass measurement capacity naturally provided by Fourier transform ion cyclotron resonance mass spectrometry(FT-ICR-MS)minimizes the matrix interferences and thus enables the evaluation of phthalates in a complex matrix without extensive sample handlings or preparations.The limits of quantification(LOQs)were estimated to be at 0.3-5.0 ng•mL^(−1),lower than the Maximum Residue Limit(MRL)regulated by the European Union legislations(2007/19/EC)in foods,beverages,food packaging and toys(0.3-30 ng•mL^(−1)).This rapid and easy-to-use SPME-DART-FT-ICR-MS method provided a relatively high-throughput and powerful analytical approach for quick testing and screening phthalates in beverages and water samples to ensure food safety.
基金supported by the fund of the Beijing Laboratory for Food Quality and Safety,Beijing Technology and Business University,China(No.FQS-201810)Science and Technology Commission of Shanghai Municipality,China(No.19DZ2284200).
文摘An analytical method using gas chromatography isotope ratio mass spectrometry(GC-IRMS)combined with solid phase micro-extraction(SPME)was developed to measure the 613C values of six typical volatiles commonly occurring in wine(isoamyl acetate,2-octanone,limonene,2-phenylethanol,ethyl octanoate and ethyl decanoate)for the first time.SPME selected with a divinylbenzene/carboxen/polydimethylsiloxane fiber was combined with the GC-IRMS for pretreatment optimization.The optimized SPME parameters of extraction time,extraction temperature and salt concentration were 40 min,40℃ and 10%,respectively.The 613C values measured by SPME-GC-IRMS were in good agreement with those measured via elemental analyzer(EA)-IRMS and GC-IRMS.The differences range from 0.02‰to 0.44‰ with EA-IRMS and from 0 to 0.28‰ with GC-IRMS,indicating the high accuracy of the method.This newly established method measured the precision within 0.30‰ and was successfully validated to discriminate imported real wine samples with identical label but amazing price differences from different importers.
