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Gas Chromatographic Method for Identification and Quantification of Commonly Used Residual Solvents in Pharmaceuticals Products
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作者 Sreekanta Nath Dalal Pranab Kumar Das 《American Journal of Analytical Chemistry》 CAS 2024年第8期241-252,共12页
Background: Impurities are not expected in the final pharmaceutical products. All impurities should be regulated in both drug substances and drug products in accordance with pharmacopeias and ICH guidelines. Three dif... Background: Impurities are not expected in the final pharmaceutical products. All impurities should be regulated in both drug substances and drug products in accordance with pharmacopeias and ICH guidelines. Three different types of impurities are generally available in the pharmaceutical’s product specification: organic impurities, inorganic impurities, and residual solvents. Residual solvents are organic volatile chemicals used or generated during the manufacturing of drug substances or drug products. Purpose: The aim of this study is to develop a cost-effective gas chromatographic method for the identification and quantification of some commonly used solvents—methanol, acetone, isopropyl alcohol (IPA), methylene chloride, ethyl acetate, tetrahydrofuran (THF), benzene, toluene, and pyridine—in pharmaceutical product manufacturing. This method will be able to identify and quantify the multiple solvents within a single gas chromatographic procedure. Method: A gas chromatography (GC) equipped with a headspace sampler and a flame ionization detector, and a column DB 624, 30-meter-long × 0.32-millimeter internal diameter, 1,8 μm-thick, Brand-Agilent was used to develop this method. The initial GC oven temperature was 40°C and held for 5 minutes. It was then increase to 80˚C at a rate of 2˚C per minute, followed by a further increase to 225˚C at a rate of 30˚C per minute, with a final hold at 225˚C for 10 minutes. Nitrogen was used as a carrier gas at a flow rate of 1.20 mL per minute. Dimethyl sulfoxide (DMSO) was selected as sample solvent. Results: The developed method is precise and specific. The percent RSD for the areas of six replicate injections of this gas chromatographic method was within 10.0 and the recovery result found within 80.0% to 120.0%. 展开更多
关键词 Method Development gas chromatography Compendial Method GDP SPECIFICITY RECOVERY
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Determination of 14 Organophosphorus Pesticide Residues in Mutton by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry(GPC-GC-MS)
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作者 Junpeng ZHAO Richard Avoi +2 位作者 Azman Bin Atil@Azmi Jiao CHEN Ling YUN 《Agricultural Biotechnology》 2024年第3期28-30,33,共4页
[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by ga... [Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton. 展开更多
关键词 MUTTON gas chromatography-mass spectrometry Gel permeation chromatography ORGANOPHOSPHORUS Pesticide residue
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Preparation of new hybrid organic/inorganic polymeric chiral stationary phases for ligand-exchange chromatography 被引量:2
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作者 Rui Juan Song Yu Fu +2 位作者 Na Yao Yuan De Long Tian Bao Huang 《Chinese Chemical Letters》 SCIE CAS CSCD 2007年第10期1250-1252,共3页
Three new hybrid organic/inorganic polymeric ligand-exchange chiral stationary phases were developed by radical chain transfer reaction and surface grafting on silica gel, and successfully used for the enantioseparati... Three new hybrid organic/inorganic polymeric ligand-exchange chiral stationary phases were developed by radical chain transfer reaction and surface grafting on silica gel, and successfully used for the enantioseparations of DL-amino acids and DL-hydroxyl adds. The resolutions were achieved by using water containing 2.0 × 10^-4 mol/L of CuAc2 as a mobile phase, column temperature of 40 ℃, flow rate of 1.0 mL/min and detection at UV 254 nm. The elution order of D-isomer before L-isomer was observed for all DL-amino acids resolved except DL-Pro. 展开更多
关键词 Chiral stationary phase ligand-exchange chromatography DL-Hydroxyl acid Surface grafting DL-Amino acid
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A chiral stationary phase with special hydrophobic framework for ligand-exchange chromatography
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作者 Hong Yu Shi Rui Juan Song +3 位作者 YU Fu Na Yao Yuan De Long Tian Bao Huang 《Chinese Chemical Letters》 SCIE CAS CSCD 2007年第11期1392-1394,共3页
A novel chiral stationary phase (CSP1) for ligand-exchange chromatography (CLEC) was prepared by firstly using dimethylchlorosilane as an endcapping reagent for decreasing residual silanol group on the surface of ... A novel chiral stationary phase (CSP1) for ligand-exchange chromatography (CLEC) was prepared by firstly using dimethylchlorosilane as an endcapping reagent for decreasing residual silanol group on the surface of silica gel, and then introducing L-Pro as a chiral selector and hydrophobic octyl group to the silica gel surface simultaneously. The enantioseparations of 14 DL-amino acids on CSP1 were achieved with the enantioselectivity α ranging from 1.09 to 2.44 and the resolution Rs being between 0.8 and 6.3. The chromatographic performances of CSP1 with the bonded phase (CSP2) prepared using reference method were compared. The results showed that the column efficiency and resolution Rs of chiral stationary phase could be improved by using the above modifying method. 展开更多
关键词 ligand-exchange chromatography Chiral stationary phase Amino acids Enantiomeric resolution
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Classification of Chinese Traditional Drug-"Beimu" (Bulbus Fritillariae) by Pyrolysis High Resolution Gas Chromatography-Pattern Recognition 被引量:2
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作者 房杏春 李萍 +1 位作者 田琳 安登魁 《Journal of Chinese Pharmaceutical Sciences》 CAS 1992年第2期65-72,共8页
The combination of pyrolysis high resolution gas chromatography and pat- tern recognition techniques is a powerful tool for the classification of traditional Chinese drug.A study has been completed on 55 Beimu samples... The combination of pyrolysis high resolution gas chromatography and pat- tern recognition techniques is a powerful tool for the classification of traditional Chinese drug.A study has been completed on 55 Beimu samples of five different geographic origins: Eastern China.Central China.South-western China,North-western China and North-eastern China.Principal component analysis and SIMCA are applied to effectively classifying the samples according to the origin of the plants.The chemical information contained in the high resolution gas chromatographic data is sufficient to characterize the geographic origin of sam- pies. 展开更多
关键词 Beimu FRITILLARIA Pyrolysis High Resolution gas chromatography Pattern Recognition
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Determination of phthalate esters in fat-containing foods by packed nanofiber solid-phase extraction column and gas chromatography 被引量:2
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作者 邱金丽 王羽 +1 位作者 周小玲 康学军 《Journal of Southeast University(English Edition)》 EI CAS 2016年第3期322-326,共5页
A new method for simultaneous determination of four phthalate esters ( PAEs) in commercial fat-containing foods was developed by the combination of a packed nanofibers column based on solid-phase extraction with gas... A new method for simultaneous determination of four phthalate esters ( PAEs) in commercial fat-containing foods was developed by the combination of a packed nanofibers column based on solid-phase extraction with gas chromatography-flame ionization detector ( GC-FID ). Conditions for obtaining optimum extraction efficiency such as extraction solvents, morphologies of adsorbent, ion strength and pH were investigated and optimized in detail. Under the optimized conditions, the limits of detection (LODs) found for dibutyl phthalate (DBP) , butyl benzyl phthalate (BBP), diethyl hexyl phthalate (DEHP) and di-n-octyl phthalate (DNOP) were 50, 25, 50 and 25 ng/g, respectively. Good linearity of four PAEs was achieved in the range of 50 to 4 000 ng/g. The proposed method was applied for analyzing different kinds of fat-containing samples. PAEs in commercial fat-containing samples can be highly extracted by a packed solid-phase extraction column of 5 mg polystyrene ( PS) nanofibers. The satisfactory average recoveries were obtained in the range of 96. 7% to 102. 3% , and the relative standard deviations (RSDs) below 5% were achieved. The proposed method reduces the organic solvent consumption, the complex and tedious procedures for sample pretreatment, and achieves high sensitivity and reproducibility for the investigated PAEs. 展开更多
关键词 phthalate esters (PAEs nanofibers solid-phase extraction gas chromatography fat-containing foods
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Determination of Dichlofluanid Residue in Soybean by Capillary Collumns Gas Chromatography 被引量:20
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作者 邵栋梁 《Agricultural Science & Technology》 CAS 2010年第3期7-8,64,共3页
A method for the determination of dichlofluanid residue by Capillary Collumns Gas Chromatography was established in this study.Samples were extracted with acetone and subjected to through liquid-liquid extraction with... A method for the determination of dichlofluanid residue by Capillary Collumns Gas Chromatography was established in this study.Samples were extracted with acetone and subjected to through liquid-liquid extraction with N-hexane,and then they were cleanup with column that filled with florisil,subsequently separated by Capillary Column Gas Chromatography,and the electron capture detector (ECD) was used for detection.The detection limit of this method was 0.005 mg/kg (S/N=3),and this method was rapid,sensitive and accurate,and was applied in the determination of dichlofluanid residue in soybean. 展开更多
关键词 Dichlofluanid Capillary Collumns gas chromatography SOYBEAN
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Separation Properties of a New Polysiloxane-Anchored β-Cyclodextrin Derivative as Gas Chromatography Stationary Phase 被引量:1
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作者 史雪岩 傅若农 顾峻岭 《Journal of Beijing Institute of Technology》 EI CAS 2002年第3期285-289,共5页
A new capillary gas chromatography stationary phase, monokis (2,6 di O benzyl 3 O propyl (3’)) hexakis(2,6 di O benzyl 3 O methyl) β CD bonded polysiloxane, was synthesized. It ex... A new capillary gas chromatography stationary phase, monokis (2,6 di O benzyl 3 O propyl (3’)) hexakis(2,6 di O benzyl 3 O methyl) β CD bonded polysiloxane, was synthesized. It exhibited separation abilities to disubstituted benzene isomers and some chiral solutes. It was also found that the polarity of CD derivatives can be lowered both by chemically bonding it to polysiloxane and by diluting it in polysiloxane. The separation abilities of the polysiloxane anchored CDs (SP CD) are higher than that of the unbonded CDs (S CD) and the diluted S CD at lower column temperature. Hydrosilylation reaction is one of the best methods to lower the operating temperature of CDs. 展开更多
关键词 capillary gas chromatography stationary phase polysiloxane anchored β cyclodextrin derivative di substituted benzene isomers separation enantiomers separation
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Pyrolysis-Gas Chromatography/Mass Spectrometry for Microstructure and Pyrolysis Pathway of Polyester-Polyether Multiblock Copolymer
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作者 罗爱芹 叶玲 +2 位作者 傅若农 谢桂阳 王显伦 《Journal of Beijing Institute of Technology》 EI CAS 2001年第1期45-50,共6页
The composition and sequence distribution of monomeric units in polyester polyether multiblock copolymer were studied by pyrolysis? gas chromatography (PGC) and pyrolysis gas chromatography/mass spectrometry (PGC/M... The composition and sequence distribution of monomeric units in polyester polyether multiblock copolymer were studied by pyrolysis? gas chromatography (PGC) and pyrolysis gas chromatography/mass spectrometry (PGC/MS). PGC was applied to study the F t curve of the multiblock copolymer and PGC/MS was used to separate and identify the pyrolyzates. DTA experiment was used to study the decomposition temperature. The results show that the beginning point of elastomer’s decomposition was about 300?℃ and the decomposition temperature of most of the sample was 550?℃. Many pyrolyzates were produced because of the breaking of weak bonds in the sample. The possible microstructure was verified and the pyrolysis pathway of the copolymer was investigated. 展开更多
关键词 thermoplastic elastomer polyester polyether multiblock copolymer pyrolysis gas chromatography/mass spectrometry copolymer pyrolysis pathway MICROSTRUCTURE pyrolyzates
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Synthesis and Characterization of Peralkylated β-Cyclodextrins Used as Gas Chromatographic Stationary Phasest
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作者 戴荣继 傅若农 +1 位作者 冯宗财 周伟 《Journal of Beijing Institute of Technology》 EI CAS 1994年第2期144-154,共11页
Six peralkylated β- cyclodec\xtrins used as capillary gas chromatographic stationary phases were prepared and characterized by differential by differential scannning calorimetry(DSC) and pyrolysis gas chromatograp... Six peralkylated β- cyclodec\xtrins used as capillary gas chromatographic stationary phases were prepared and characterized by differential by differential scannning calorimetry(DSC) and pyrolysis gas chromatography (PyGC). The DSC profiles illustrated that the peralkylated β-cyclodextrins synthesized possess the supercoooled state and the glass state below their melting point The PYGC results showed that the long-chain alkylated β-cyclodextrins are more thermostable than the short-chain. one All ofthese peralkylated β-cyclodextrins are suitable for use as capillary column gas chromatographic stationary phases,which can easily be coatal on the fused silica capilary columns and have nice chromatographic retention behaviour. For example, the capillary colunns coated with these materials can excellently separate three methylphenol isomers and six dimehylphenol isomers. 展开更多
关键词 CYCLODEXTRIN gas chromatography/peralkylated cyclodextrin
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Application of Pyrolysis-Gas Chromatography in Explosive and Propellant Analysis
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作者 刘虎威 傅若农 《Journal of Beijing Institute of Technology》 EI CAS 1992年第1期13-18,共6页
Applications of pyrolysis-gas chromatography and pyrolysis capillary gas chromatography in explosive and propellant analysis are reviewed, including the identification of explosives and propel- lants, the investigatio... Applications of pyrolysis-gas chromatography and pyrolysis capillary gas chromatography in explosive and propellant analysis are reviewed, including the identification of explosives and propel- lants, the investigation of the thermal decomposition of nitrocellulose (NC), cyclotetramethylene tetranitramine (HMX)and cyclotrimethylene trinitramine (RDX), and the study of the wear- reducing mechanism of polyurethane additive in propellant gain. 展开更多
关键词 gas chromatography explosives propellant/pyrolysis-gas chromatography
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Enantioselective Determination of R-(-)-and S-(+)-Mexiletine in Microsomal Incubates by Capillary gas Chromatography
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作者 王似菊 毛海琼 曾苏 《Journal of Chinese Pharmaceutical Sciences》 CAS 1998年第4期34-37,共4页
A method for the assay of R ( ) and S (+) mexiletine in rat liver microsomal incubates was developed. The method involved extraction of mexiletine from the microsomal incubates, and formation of mexiletine diast... A method for the assay of R ( ) and S (+) mexiletine in rat liver microsomal incubates was developed. The method involved extraction of mexiletine from the microsomal incubates, and formation of mexiletine diastereomeric derivatives with a chiral reagent S ( ) N trifluoroacetyl prolyl chloride. Separation and quantitation of the diastereomeric mexiletine derivatives were carried out by a capillary gas chromatographic system with flame ionization detection. The assay was linear from 5 to 500 μg/ml for each enantiomer. The average recoveries of analytical method were 93 31±5 59% and 93 10±5 11% for R ( ) and S (+) mexiletine, respectively. The limits of detection and quantitation for the method were 1 0 μg/ml and 5 0 μg/ml for the R ( ) and S (+) mexiletine isomers, respectively. The reproducibility in the assay was better than 16.5% (RSD). The method has been applied to the metabolism study of R ( ) and S (+) mexiletine in rat liver microsomal incubates. 展开更多
关键词 MEXILETINE Capillary gas chromatography Enantiomer separation
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Cross-Linked Crown Ether-SE-54 as Stationary Phase for Open-Tubular Column Gas Chromatography
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作者 朱荣萍 傅若农 +4 位作者 葛继龙 王宏菊 朱济亚 黄载福 张斌 《Journal of Beijing Institute of Technology》 EI CAS 1992年第2期87-93,共7页
The cross-linking of crown ether-SE-54 in fused-silica capillary columns were initiated by dicumyl peroxide(DCUP),azo-bis-isobutyronitrile (AIBN)and ozone(O_3).Parameters of evaluation such as polarity,selectivity, ph... The cross-linking of crown ether-SE-54 in fused-silica capillary columns were initiated by dicumyl peroxide(DCUP),azo-bis-isobutyronitrile (AIBN)and ozone(O_3).Parameters of evaluation such as polarity,selectivity, phase transition temperature and thermal stability were studied and compared with those of poly(crown ether)stationary phase. 展开更多
关键词 gas chromatography crosslinking/capillary gas chromatography crown ether poly(crown ether)
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Metabolomics of gastric cancer metastasis detected by gas chromatography and mass spectrometry 被引量:13
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作者 Jin-Lian Chen,Jun-Duo Hu,Jing Fan,Jing Hong,Department of Gastroenterology,Shanghai Sixth People’s Hospital,Shanghai Jiao Tong University,Shanghai 200233,China Hui-Qing Tang,Jian-Zhong Gu,Shanghai Laboratory Animal Center,Chinese Academy of Sciences,Shanghai 201615,China 《World Journal of Gastroenterology》 SCIE CAS CSCD 2010年第46期5874-5880,共7页
AIM:To elucidate the underlying mechanisms of metastasis and to identify the metabolomic markers of gastric cancer metastasis.METHODS:Gastric tumors from metastatic and nonmetastatic groups were used in this study.Met... AIM:To elucidate the underlying mechanisms of metastasis and to identify the metabolomic markers of gastric cancer metastasis.METHODS:Gastric tumors from metastatic and nonmetastatic groups were used in this study.Metabolites and different metabolic patterns were analyzed by gas chromatography,mass spectrometry and principal components analysis (PCA),respectively.Differentiation performance was validated by the area under the curve (AUC) of receiver operating characteristic curves.RESULTS:Twenty-nine metabolites were differentially expressed in animal models of human gastric cancer.Of the 29 metabolites,20 were up-regulated and 9 were down-regulated in metastasis group compared to non-metastasis group.PCA models from the metabolite profiles could differentiate the metastatic from the nonmetastatic specimens with an AUC value of 1.0.These metabolites were mainly involved in several metabolic pathways,including glycolysis (lactic acid,alaline),serine metabolism (serine,phosphoserine),proline metabolism (proline),glutamic acid metabolism,tricarboxylic acid cycle (succinate,malic acid),nucleotide metabolism (pyrimidine),fatty acid metabolism (docosanoic acid,and octadecanoic acid),and methylation(glycine).The serine and proline metabolisms were highlighted during the progression of metastasis.CONCLUSION:Proline and serine metabolisms play an important role in metastasis.The metabolic profiling of tumor tissue can provide new biomarkers for the treatment of gastric cancer metastasis. 展开更多
关键词 gasTRIC cancer METASTASIS METABOLITE Metabolomics gas chromatography and mass SPECTROMETRY
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Gas chromatography/mass spectrometry based metabolomic study in a murine model of irritable bowel syndrome 被引量:8
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作者 Lei-Min Yu Ke-Jia Zhao +2 位作者 Shuang-Shuang Wang Xi Wang Bin Lu 《World Journal of Gastroenterology》 SCIE CAS 2018年第8期894-904,共11页
AIM To study the role of microbial metabolites in the modulation of biochemical and physiological processes in irritable bowel syndrome(IBS).METHODS In the current study, using a metabolomic approach, we analyzed the ... AIM To study the role of microbial metabolites in the modulation of biochemical and physiological processes in irritable bowel syndrome(IBS).METHODS In the current study, using a metabolomic approach, we analyzed the key metabolites differentially excreted in the feces of control mice and mice with IBS, with or without Clostridium butyricum(C. butyricum) treatment. C57 BL/6 mice were divided into control, IBS, and IBS + C. butyricum groups. In the IBS and IBS + C. butyricum groups, the mice were subjected to water avoidance stress(WAS) for 1 h/d for ten days. Gas chromatography/mass spectrometry(GC-MS) together with multivariate analysis was employed to compare the fecal samples between groups. RESULTS WAS exposure established an appropriate model of IBS in mice, with symptoms of visceral hyperalgesia and diarrhea. The differences in the metabolite profiles between the control group and IBS group significantly changed with the progression of IBS(days 0, 5, 10, and 17). A total of 14 differentially excreted metabolites were identified between the control and IBS groups, and phenylethylamine was a major metabolite induced by stress. In addition, phenylalanine metabolism was found to be the most relevant metabolic pathway. Between the IBS group and IBS + C. butyricum group, 10 differentially excreted metabolites were identified. Among these, pantothenate and coenzyme A(Co A) biosynthesis metabolites, as well as steroid hormone biosynthesis metabolites were identified as significantly relevant metabolic pathways.CONCLUSION The metabolic profile of IBS mice is significantly altered compared to control mice. Supplementation with C. butyricum to IBS mice may provide a considerable benefit by modulating host metabolism. 展开更多
关键词 IRRITABLE BOWEL syndrome METABOLITE gas chromatography/mass spectrometry CLOSTRIDIUM butyricum
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Detection of Tocopherol in Oilseed Rape (Brassica napus L.) Using Gas Chromatography with Flame Ionization Detector 被引量:6
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作者 Nazim Hussain Zahra Jabeen +6 位作者 LI Yuan-long CHEN Ming-xun LI Zhi-lan GUO Wan-li Imran Haider Shamsi CHEN Xiao-yang JIANG Li-xi 《Journal of Integrative Agriculture》 SCIE CAS CSCD 2013年第5期803-814,共12页
The variation among Chinese genotypes of Brassica napus L. for seed tocopherols content and their analysis using gas chromatography has not been comprehensively reported till to date. In the present study, the tocophe... The variation among Chinese genotypes of Brassica napus L. for seed tocopherols content and their analysis using gas chromatography has not been comprehensively reported till to date. In the present study, the tocopherol contents of four Chinese genotypes of Brassica napus L., namely, Gaoyou 605, Zhejiang 619, Zheshuang 758, and Zheshuang 72, were evaluated using three modified sample preparation protocols (P1, P2, and P3) for tocopherol extraction. These methods were distinguished as follows. Protocol one (P1) included the evaporation of solvent after extraction without silylation. Protocol two (P2) followed the direct supernatant collection after overnight extraction without drying and silylation. Protocol three (P3) included trimethylsilylation with N,O-bis(trimethylsilyl) trifluoroacetamide. Genotypic comparison of tocopherol and its isoforms revealed that Gaoyou 605 was dominant over the other genotypes with (140.5+ 10.5), (316.2+ 9.2), and (559.1+ 24.3) ~tg g-~ of seed meal ct-, 7-, and total (T-) tocopherol, respectively, and a 0.44+0.04 ^- to 7-tocopherol ratio. The comparison of the sample preparation protocols, on the other hand, suggests that P3 is the most suitable method for the tocopherol extraction from Brassica oilseeds and for the analysis of tocopherols using gas chromatography flame ionization detector (GC-FID). Trimethylsilylation is the key step differentiating P3 from P1 and P2. Variations detected in tocopherol contents among the Chinese rapeseed (B. napus) genotypes signify the need to quantify a wide range of rapeseed germplasm for seed tocopherol dynamics in short and crop improvement in long. 展开更多
关键词 Brassica napus L. genotypic variation tocopherol analysis gas chromatography flame ionization detector
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Chromatoprobe as a sample-sparing technique for residual solvent analysis of drug discovery candidates by gas chromatography 被引量:3
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作者 Christopher J.Poronsky Jingfang Qian Cutrone 《Journal of Pharmaceutical Analysis》 SCIE CAS CSCD 2017年第4期265-269,共5页
In drug discovery research, residual solvent measurement is an integral part of purity analysis for synthesis of a drug candidate before it is used for toxicity testing. This is usually carried out using gas chromatog... In drug discovery research, residual solvent measurement is an integral part of purity analysis for synthesis of a drug candidate before it is used for toxicity testing. This is usually carried out using gas chromatography(GC)with direct injection sample introduction. This method requires testing compounds to be soluble at high concentrations( > 50 mg/mL, usually in DMSO) to achieve acceptable sensitivity, a hurdle which is not always achievable for some samples such as cyclic peptides and oligonucleotides. To overcome the limitation associated with the direct injection approach, a new method using the Chromatoprobe thermal extraction device was developed for quantifying residual solvents of drug discovery compounds. This method not only consumes significantly less material(less than 1 mg), but also shows higher sensitivity than the direct injection approach.In addition, because no diluent is required with the Chromatoprobe thermal extraction, all residual solvents can be detected and measured without further method optimization. In our study, we compared data from GC residual solvent analysis using the Chromatoprobe solid sample introduction to those of the direct injection method for seven in-house samples. Our results showed a good agreement between the data from these two sample introduction methods. Thus, the Chromatoprobe sample introduction method provided a samplesparing alternative to the direct injection method for the measurement of residual solvents in drug discovery.This method can be particularly useful for residual solvent analysis in samples that are available only in limited amounts, poorly soluble, and/or unstable in the diluents used for the direct injection method. 展开更多
关键词 Chromatoprobe Thermal extraction gas chromatography RESIDUAL SOLVENT DRUG discovery
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A study on α-ketoadipic aciduria by gas chromatographic-mass spectrometry 被引量:3
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作者 Yoshito Inoue Morimasa Ohse +1 位作者 Toshihiro Shinka Tomiko Kuhara 《World Journal of Gastroenterology》 SCIE CAS CSCD 2000年第5期766-769,共4页
INTRODUCTIONα-ketoadipate(α-KA),an intermediate in thecatabolism of L-lysine,hydroxylysine,and L-tryptophan,undergoes oxidative deearboxylation toform glutaryl-CoA and then dehydrogenates to formcrotonyl-CoA,the lat... INTRODUCTIONα-ketoadipate(α-KA),an intermediate in thecatabolism of L-lysine,hydroxylysine,and L-tryptophan,undergoes oxidative deearboxylation toform glutaryl-CoA and then dehydrogenates to formcrotonyl-CoA,the latter undergoes furtherdegradation and enters in TCA cycle,as shown inFigure 1.α-ketoadipic aciduria (Mckusick 245130)is a rare inborn error in the metabolism of α-KA 展开更多
关键词 L-LYSINE hydroxylysine Ltryptophan alpha-aminoadipic alpha-ketoadipic aciduria metabolism INBORN error mass fragmentography chromatography gas
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Measurement of Infinite Diluted Activity Coefficient of Solvents in Polymer by Inverse Gas Chromatography Method 被引量:4
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作者 冯媛媛 叶汝强 刘洪来 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2000年第2期167-170,共4页
The infinite diluted activity coefficients of solvents in polyisopropyl methylacrylate was measured using inverse gas chromatography. The solvents used were benzene, toluene, ethyl benzene, methyl acetate, ethyl aceta... The infinite diluted activity coefficients of solvents in polyisopropyl methylacrylate was measured using inverse gas chromatography. The solvents used were benzene, toluene, ethyl benzene, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methanol, ethanol isopropyl alcohol, butyl alcohol, 1,2-dichloroethane, and chloroform. It was observed that the infinite diluted activity coefficient of alcohols are well above those of the other solvents investigated. 展开更多
关键词 infinite diluted activity coefficient inverse gas chromatography specific retention volume poly(isopropyl methacrylate) THERMODYNAMICS
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Determination of Eight Organophosphorus Pesticide Residues in Pepper by QuEChERS-Gas Chromatography 被引量:7
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作者 Siyuan BI Zhiqiang ZHU +3 位作者 Wenhua CHI Mingshan CHEN Xingxing WANG Shouan ZHOU 《Agricultural Biotechnology》 CAS 2018年第1期123-125,共3页
[ Objectives] This study was conducted to establish a QuEChERS-gas chromatography method for determination of eight kinds of organophosphorus pesticide residues in pepper. [Methods] The samples were extracted by aceto... [ Objectives] This study was conducted to establish a QuEChERS-gas chromatography method for determination of eight kinds of organophosphorus pesticide residues in pepper. [Methods] The samples were extracted by acetonitrile, and anhydrous magnesium sulfate was used for salting out. The extracts were then purified by dispersive solid phase extraction combining with GCB, C18 and PSA. Samples were analyzed by FPD detector. External standard was used as quantitive method. [ Results] The detection limits were in the range of 0. 001 -0. 008 mg/kg, the average recoveries ranged from 83.5% to 101.2% , and the relative standard deviation (RSD) of the eight organophosphorus pesticide residues were below 5%. [ Conclusions] The method is simple, quick, easy and effective for the determination of pepper. 展开更多
关键词 QUECHERS gas chromatography PEPPER ORGANOPHOSPHORUS Pesticide residues
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