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91.
Analysis of amino acids by gas chromatography-mass spectrometry (GC–MS) requires at least one derivatization step to enable solubility in GC–MS-compatible water-immiscible organic solvents such as toluene, to make them volatile to introduce into the gas chromatograph and thermally stable enough for separation in the GC column and introduction into the ion-source, and finally to increase their ionization by increasing their electronegativity using F-rich reagents. In this work we investigated the long-term stability of the methyl esters pentafluoropropionic (Me-PFP) derivatives of 21 urinary amino acids prepared by a two-step derivatization procedure and extraction by toluene. In situ prepared trideuteromethyl ester pentafluoropropionic derivatives were used as internal standards. GC–MS analysis (injection of 1 µL aliquots and quantification by selected-ion monitoring of specific mass fragments) was performed on days 1, 2, 8, and 15. Measured peak areas and calculated peak area ratios were used to evaluate the stability of the derivatives of endogenous amino acids and their internal standards, as well as the precision and the accuracy of the method. All analyses were performed under routine conditions. Me-PFP derivatives of endogenous amino acids and their stable-isotope labelled analogs were stable in toluene for 14 days. The peak area values of the derivatives of most amino acids and their internal standards were slightly higher on days 8 and 15 compared to days 1 and 2, yet the peak area ratio values of endogenous amino acids to their internal standards did not change. Our study indicates that Me-PFP derivatives of amino acids from human urine samples can easily be prepared, are stable at least for 14 days in the extraction solvent toluene, and allow for precise and accurate quantitative measurements by GC–MS using in situ prepared deuterium-labelled methyl ester as internal standard. 相似文献
92.
《印度化学会志》2021,98(3):100027
The convenient route for the synthesis of a series of new Isoindoline-1, 3-dione/phthalimide analogues by condensation of substituted phthalic anhydride with an appropriate Ar-amine is described. Selective phthalimide derivatives were evaluated for their preliminary biological activities against Gram-positive, Gram-negative and fungi strains. These encouraging results could be helpful for the development of new antibacterial or antifungal agents. 相似文献
93.
Srinivas Cheruku Chaithra Nagaraju Poornima Shetty Swarup Hassan A Sandhya Nagarakere C 《合成通讯》2020,50(10):1486-1494
AbstractWe have developed an economical and efficient method for the synthesis of medicinally and synthetically important indole-based triarylmethanes by using indoles and benzhydrols in the presence of propylphosphonic anhydride (T3P®). This methodology is an alternate approach for the C–C bond formation with good to excellent yields. In this T3P-mediated dehydration approach, the by-product is highly soluble in water, so that it can be done at larger scale also. In addition to that this efficient protocol has several advantages such as mild reaction conditions, short reaction time and operational simplicity. We have successfully synthesized pyrrole, imidazothiadiazole and imidazolo pyridine based triarylmethanes also. 相似文献
94.
以碳酸二甲酯(DMC)代替光气,一锅法合成α-氨基酸-N-羧酸酐(NCAs)是实现绿色制备多肽的重要途径.制备了酸碱协同催化剂NaZnPO4,用该催化剂催化DMC和丙氨酸"一锅法"合成N-羧基丙氨酸酸酐(Ala-NCA).在N,N-二甲基甲酰胺(DMF)溶剂中,150℃的反应条件反应8 h时,Ala-NCA的收率最高为46.84%,催化剂循环5次后收率仍达38.62%.NaZnPO4中Zn2+和O-Na具有有效的酸碱协同催化作用,在反应过程中具有去质子化、精准酰基化和高效成环的作用.利用TG-MS-IR技术研究了催化剂表面上原料转化和中间体精准关环过程,并提出了可能的反应催化机理. 相似文献
95.
Xuefang Liu Chen Yang Feifang Zhang Huiliang Geng Bingcheng Yang 《Journal of separation science》2020,43(8):1474-1478
A novel weak cation exchanger is described by encapsulating silica with a (or multiple) layer(s) of maleic anhydride–modified polyvinyl alcohol coating(s). The preparation method is facile and fast, which is simply performed by dipping silica particles into maleic anhydride–modified polyvinyl alcohol solution as‐synthesized, then filtering and curing thermally, and finally generating a thin coating onto silica particles. Multiple layers of maleic anhydride–modified polyvinyl alcohol coatings can be generated by repeating above steps, offering an easy way to manipulate the capacity. The obtained weak cation exchanger demonstrated high separation efficiency and good selectivity toward common inorganic cations, for example, high plate count of 81 000 per meter was obtained for NH4+. Simultaneous separation of alkali and alkaline earth metals could be achieved within 14 min under isocratic conditions. 相似文献
96.
Monitoring of estradiol and its metabolites in biological samples is essential for the accurate diagnosis of a number of endocrine diseases. In this study, a sensitive, precise and specific GC–MS/MS method for the quantification of 17β-estradiol (17-BE) and its main metabolite, 2-methoxyestradiol (2-MEOE), in plasma was developed and validated. Plasma concentrations of these steroids are currently investigated as diagnostic markers for pre-eclampsia, a systematic disorder of pregnancy and a leading cause of maternal and fetal morbidity and mortality worldwide. 相似文献
97.
Yo Hiranoi Miho Hatanaka Koji Nakano 《Journal of polymer science. Part A, Polymer chemistry》2017,55(13):2150-2159
Di‐ and trinuclear cobalt (Co)–salen complexes with a benzene ring as a rigid linker were explored for epoxide polymerizations. The dinuclear Co–salen complex with a 1,2‐phenylene linker showed higher catalytic activity than the dinuclear Co–salen complex with a 1,3‐phenylene linker and the trinuclear Co–salen complex with a 1,3,5‐benzenetriyl linker for the copolymerization of propylene oxide (PO) with carbon dioxide. A combination of the absolute configuration of the two Co–salen moieties was found to affect its catalytic activity. The optimized dinuclear Co–salen complex with a heterochiral combination demonstrated highest activity and maintained its catalytic activity under a low catalyst concentration. The heterochiral dinuclear Co–salen complex also showed high activity for the copolymerization of PO with cyclic anhydride. © 2017 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017 , 55, 2150–2159 相似文献
98.
A novel approach to the synthesis of 4-phenylethynylphthalic anhydride has been described.The target compound was synthesized by Pd/Cu catalyzed Sonogashira coupling reaction between phenylacetylene and 4-bromophthalic acid which was for the first time employed as start material,followed by dehydration of 4-phenylethynylphthalic acid.Compared with traditional synthetic routes,this method provides several advantages such as readily available raw materials,convenient manipulation and high yield.The product... 相似文献
99.
SUI XinCe SHI Yan & FU ZhiFeng State Key Laboratory of Chemical Resource Engineering Beijing University of Chemical Technology Beijing China 《中国科学B辑(英文版)》2011,(3)
A novel copolymer network with acetal structure was prepared using bis[4-(vinyloxy)butyl](4-methyl-1,3-phenylene)biscarbamate(BECT)as the crosslinking agent.Firstly,a tri-copolymer of maleic anhydride(MAn),n-butyl vinyl ether(BVE)and 4-hydroxybutyl vinyl ether(HBVE)was synthesized via free-radical polymerization with 2,2′-azobisisobutyronitrile as the initiator.The tri-copolymer consisted of two sorts of alternating units,MAn-alt-BVE and MAn-alt-HBVE.The linear copolymer Poly((MAn-alt-BVE)-co-(MAn-alt-HBVE)... 相似文献
100.
John Kallikat Augustine Rajesha KumarAgnes Bombrun Ashis Baran Mandal 《Tetrahedron letters》2011,52(10):1074-1077
An efficient method for the Beckmann rearrangement of ketoximes to amides mediated by a catalytic amount (15 mol %) of propylphosphonic anhydride (T3P®) is described. Aldoximes underwent second order Beckmann rearrangement to provide the corresponding nitriles in excellent yields on reacting with T3P (15 mol %) at room temperature. The main advantages of this environmentally friendly protocol include procedural simplicity, and particularly ease of isolation of the products. 相似文献