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微波水解衍生高效液相色谱法测定西洋参中的氨基酸 总被引:3,自引:0,他引:3
用微波辅助提取酸水解西洋参中的蛋白质, 对生成的氨基酸进行微波衍生后用高效液相色谱法进行测定.对微波衍生条件和微波水解的条件进行了优化.研究结果表明, 190 ℃, 15 min微波水解得到氨基酸的产率与传统加热水解(110 ℃, 24 h)的结果基本相同.用2,4-二硝基氟苯(DNFB)对氨基酸进行微波衍生, 氨基酸在微波衍生时间大于20 s时, 衍生反应基本完全; 而传统DNFB衍生需在60 ℃水浴加热1 h, 所以微波衍生法明显缩短了氨基酸分析时间.用高效液相色谱法对西洋参根中的氨基酸进行了测定, 结果令人满意. 相似文献
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以2-N-(N’-苄基脯氨酰)-氨基二苯甲酮-镍(II)-丙基酸复合物为手性助剂, 与不同碳链长度的二溴烷烃反应制备 双-α-甲基氨基酸. 其中, BPB-Ni(II)-Ala复合物与1,3-二溴丙烷发生取代-消除反应后生成烯丙基取代复合物中间体, 产率高达90%, 水解生成2-甲基-2-氨基-4-烯-戊酸; 与1,4-二溴丁烷、1,5-二溴戊烷、1,6-二溴己烷可以实现双取代反应, 但所得的主要产物为单取代的BPB-Ni(II)-Ala复合物, 双-α-甲基氨基酸复合物中间体收率分别为38%, 36%, 45%, 经过水解后生成相应的双-α-甲基氨基酸, 分别为2,7-二氨基-2,7-二甲基辛二酸、2,8-二氨基-2,8-二甲基壬二酸、2,9-二氨基-2,9-二甲基癸二酸. 手性助剂2-N-(N’-苄基脯氨酰)-氨基二苯甲酮的回收率可高达95%. 相似文献
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以2-N-(N'-苄基脯氨酰)-氨基二苯甲酮-镍(Ⅱ)-丙基酸复合物为手性助剂,与不同碳链长度的二溴烷烃反应制备双-α-甲基氨基酸.其中,BPB-Ni(Ⅱ)-Ala复合物与1,3-二溴丙烷发生取代-消除反应后生成烯丙基取代复合物中间体,产率高达90%,水解生成2-甲基-2-氨基-4-烯-戊酸;与1,4-二溴丁烷、1,5-二溴戊烷、1,6-二溴己烷可以实现双取代反应,但所得的主要产物为单取代的BPB-Ni(Ⅱ)-Ala复合物,双-α-甲基氨基酸复合物中间体收率分别为38%,36%,45%,经过水解后生成相应的双-α-甲基氨基酸,分别为2,7-二氨基-2,7-二甲基辛二酸、2,8-二氨基-2,8-二甲基壬二酸、2,9-二氨基-2,9-二甲基癸二酸.手性助剂2-N-(N'-苄基脯氨酰)-氨基二苯甲酮的回收率可高达95%. 相似文献
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在固液两相条件下用手性季铵盐为相转移催化剂,邻苯二甲酰亚胺钾与α-溴代羧酸酯反应,合成了十二个具有光学活性的α-(邻苯二甲酰亚胺基)羧酸酯,经肼解和水解,得到相应的光学活性α-氨基酸,光学纯度百分率为3.6—17.8%。 相似文献
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研究了微波萃取烟草中游离氨基酸和微波水解烟草蛋白质的样品前处理方法,对微波萃取和微波水解条件进行了优化。微波萃取后的游离氨基酸及微波水解后的氨基酸总量采用氨基酸分析仪测定,蛋白质中的氨基酸用差减法计算。微波萃取氨基酸的最佳条件为:盐酸浓度0.05 mol·L-1,物料比1∶20,微波萃取温度50℃,微波萃取时间10 min,该条件下得到的游离氨基酸萃取率与超声30 min的结果基本一致;微波水解蛋白质的最佳条件为:盐酸浓度6 mol·L-1,物料比1∶100,水解温度140℃,水解时间60 min,与传统水解24 h的结果基本一致。用微波辅助法萃取烟草中的游离氨基酸及水解烟草蛋白质,样品前处理时间大大缩短,分析结果令人满意。 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
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A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
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A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions. 相似文献