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王东武王西宁宋莹雪肖海敏 《理化检验(化学分册)》2015,(10):1358-1363
建立了测定琥珀酸索利那新原料药中残留溶剂甲醇、乙醇、丙酮、叔丁醇、乙酸乙酯、正庚烷、石油醚、甲苯的气相色谱法和测定吡啶的高效液相色谱法。气相色谱法中以N,N-二甲基甲酰胺为溶剂,以TR-5毛细管柱为分离柱,采用氢火焰离子化检测器。高效液相色谱法中以AQC18色谱柱为分离柱,以50mmol·L-1磷酸氢二钠水溶液(含0.1%三乙胺,pH为7.6)-乙腈(1+1)为流动相,检测波长为254nm。9种溶剂的质量浓度在一定范围内呈线性,吡啶的检出限为0.01mg·L-1,其余8种溶剂的检出限在1.17~5.00 mg·L-1之间,加标回收率在86.3%~101%之间,相对标准偏差(n=6)在2.4%~6.3%之间。 相似文献
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《理化检验(化学分册)》2015,(10)
建立了测定琥珀酸索利那新原料药中残留溶剂甲醇、乙醇、丙酮、叔丁醇、乙酸乙酯、正庚烷、石油醚、甲苯的气相色谱法和测定吡啶的高效液相色谱法。气相色谱法中以N,N-二甲基甲酰胺为溶剂,以TR-5毛细管柱为分离柱,采用氢火焰离子化检测器。高效液相色谱法中以AQC18色谱柱为分离柱,以50mmol·L-1磷酸氢二钠水溶液(含0.1%三乙胺,pH为7.6)-乙腈(1+1)为流动相,检测波长为254nm。9种溶剂的质量浓度在一定范围内呈线性,吡啶的检出限为0.01mg·L-1,其余8种溶剂的检出限在1.17~5.00 mg·L-1之间,加标回收率在86.3%~101%之间,相对标准偏差(n=6)在2.4%~6.3%之间。 相似文献
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采用Oasis HLB固相萃取柱萃取水中灭多威肟,建立了固相萃取高效液相色谱法测定水中灭多威肟的分析方法。首先用10 mL甲醇和10 mL超纯水活化Oasis HLB固相萃取柱,以1 mL/min的流速萃取100 mL水样,用10 mL甲醇洗脱,浓缩洗脱液至1 mL后采用液相色谱法测定,甲醇–水(35∶65)为流动相,检测波长为230 nm。该方法检出限为0.14μg/L,测定结果的相对标准偏差为1.41%~2.08%,平均回收率为86.8%~88.4%。该法适用于工业废水中灭多威肟的测定。 相似文献
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建立了高效液相色谱(HPLC)-二极管阵列检测器(DAD)检测聚碳酸酯水桶中6种酚类物质的分析方法。比较了不同的提取方式和提取溶剂对目标物的提取效果,并考察了方法的线性、精密度、回收率。结果表明,采用有机溶剂溶解沉淀法,以甲醇为提取溶剂,对6种酚类物质的提取效果最佳。以甲醇-水为流动相,采用梯度洗脱的方式进行HPLC-DAD检测。目标物在0.01~5.0 mg/L范围内呈良好的线性关系,方法平均回收率在86%~99%,相对标准偏差为2.5%~6.2%。方法可用于聚碳酸酯水桶中酚类物质的实际检测。 相似文献
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采用气相色谱法和高效液相色谱法两种方法分别对克菌丹和灭菌丹进行定性定量分析。气相色谱法均以邻苯二甲酸二戊酯为内标物,色谱柱采用3%OV-101 chromosorb AW DMCS 150~177μm,1 m×3 mm玻璃柱,柱温为195℃,汽化温和检测温均为230℃,克菌丹和灭菌丹的回收率分别为99.2%~100.7%和98.8%~99.9%;方法相对标准偏差分别为0.46%和0.59%。高效液相色谱法中使用Nova-PaK C18250 mm×4.6 mm色谱柱,以V(甲醇)∶V(水)=85∶15为流动相,检测波长为225 nm。克菌丹和灭菌丹的回收率分别为99.5%~100.6%和98.9%~99.7%;方法相对标准偏差分别为0.68%和0.51%。 相似文献
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采用高效液相色谱法对己.福水分散粒剂的分析方法进行研究,色谱条件为:流动相V(甲醇)∶V(水)=75∶25,流速0.8 mL/min,保留时间在0~10min,检测波长为320 nm,10~20 min检测波长为223 nm。测定方法中己唑醇和福美双的回收率分别为98.6%~100.2%和98.6%~100.5%,相对标准偏差分别为0.53%和0.57%;悬浮率的测定方法中己唑醇、福美双的回收率分别为97.3%~99.5%、97.2%~99.7%,相对标准偏差分别为1.11%、1.46%。 相似文献
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提出了反相高效液相色谱法同时测定土壤中氰溴甲苯的方法。样品采用索氏提取法,以二氯甲烷为提取溶剂提取6 h。提取液以ODS-C18色谱柱(150 mm×6 mm,5μm)为分离柱,以甲醇-水(70+30)为流动相经色谱分离,在检测波长为237 nm处进行测定。氰溴甲苯的质量浓度在0.6~10.0 mg.L-1范围内与其峰面积呈线性关系。标准加入回收率在85.0%~95.7%之间,相对标准偏差(n=6)在1.9%~10.3%之间。 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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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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《Tetrahedron》2014,70(21):3377-3384
The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative. 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