共查询到20条相似文献,搜索用时 46 毫秒
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凝胶渗透色谱净化一气相色谱分离同时测定糙米中50种有机磷农药残留 总被引:7,自引:0,他引:7
研究了同时检测糙米中50种有机磷农药残留的方法。用乙酸乙酯提取,凝胶渗透色谱净化,环己烷-二氯甲烷(50:50,V/V)作为流动相,气相色谱-氮磷检测器检测。方法检出限为0.001~0.089mg/kg;相对标准偏差为1.7%~18.9%;40多种农药平均回收率在70%~120%。 相似文献
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反相高效液相色谱检测丹参药材中4种丹参酮的含量 总被引:6,自引:0,他引:6
建立了测定丹参药材中4种丹参酮含量的反相高效液相色谱法,色谱条件:流动相为水(含0.5%三乙胺)-甲醇-四氢呋喃(45/55/5,V/V/V),流速为1mL/min;PDA检测波长254m;4种成分丹参酮Ⅰ、丹参酮ⅡA、隐丹参酮和二氢丹参酮的加样回收率在95.1%-101.2%之间,线性范围为0.08-2μg。该方法准确,稳定,重现性好。根据该色谱条件,测定了不同产地的丹参药材,结果表明:该色谱方法准确检测了生药中4种丹参酮的含量,适合于丹参药材的质量控制。 相似文献
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研究了以麦秆为原料用水解-氧化-水解法制取草酸的工艺方法。最佳反应条件:麦秆用量50g,硫酸浓度70%,物料浸泡时间≥3h,m(硝酸):m(麦秆)=2.1:1.0;氧化催化剂V2O5-FeCl3[n(V2O5):n(FeCl3)=1:1]用量0.1g,氧化-水解反应时间5h,反应温度65℃~70℃,草酸二水合物收率75.5%。 相似文献
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柱前衍生化高效液相色谱荧光检测法测定桑叶中的1-脱氧野尻霉素 总被引:10,自引:0,他引:10
建立了芴甲氧酰氯(FMOC—Cl)柱前荧光衍生一高效液相色谱法测定桑叶中1-脱氧野尻霉素(DNJ)的方法。桑叶经0.05mol/L,盐酸提取,在pH8.5的硼酸盐缓冲溶液条件下,DNJ反应生成荧光产物,然后用高效液相色谱-荧光检测器测定。流动相为乙腈-0.1%醋酸(55:45,V/V)。线性范围为0.567~34mg/L(相关系数r=0.9999);检出限为0.03mg/L。实验测得桑叶中DNJ含量为0.24%;平均回收率为97.1%,RSD为1.35%(n=6)。 相似文献
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高效液相色谱法测定灯盏花制剂中灯盏乙素含量 总被引:3,自引:0,他引:3
建立了高效液相色谱法(HPLC)测定灯盏花制剂中灯盏乙素含量的方法,运用二极管阵列检测器(PDA)进行光谱分析确认灯盏乙素,采用C18反相柱,以乙腈:水:醋酸(HAC):2%磷酸(H3PO4)=20.0:77.5:2.0:0.5(V/V)为流动相测定了同一批灯盏花素片剂中灯盏乙素,含量为12.53%,标准偏差0.63,变异系数5.03%,回收率为100.17%.方法快速,精密度及准确度在允许范围内. 相似文献
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以糠醛和乙酸酐为原料,聚乙二醇为相转移催化剂,在微波辐射下合成了α-呋喃丙烯酸。较适宜的反应条件为:糠醛10mL(122mmol),V(糠醛):V(乙酸酐)=1:2,n(糠醛):n(K2CO3)=1:0.55,PEG1000用量为糠醛质量的4.3%,微波辐射功率260w,辐射时间11min,产率72.3%。 相似文献
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以对氨基苯磺酰胺、丙烯酰氯(或甲基丙烯酰氯)为原料合成了N-[4-(磺酰胺)苯基]丙烯酰胺(ASPAA)和N-[4-(磺酰胺)苯基]甲基丙烯酰胺(ASPMAA),其结构经^1H NMR,IR和元素分析表征。合成ASPAA的最佳条件:对氨基苯磺酰胺13.76g(80mmol),n(对氨基苯磺酰胺):n(丙烯酰氯)=1.0:1.1,n(丙烯酰氯):n(NaHCO3):1.00:1.14,0℃~2℃反应3h,反应液倾入10倍体积的的甲醇-水[V(甲醇):V(水)=1:10]中析出产物,收率在60%以上。合成ASPMAA的最佳条件:对氨基苯磺酰胺6.88g(40mmol),n(对氨基苯磺酰胺):n(甲基丙烯酰氯)=1.00:1.05,n(三己胺):n(甲基丙烯酰氯):1.0:1.0,在0℃~2℃滴加甲基丙烯酰氯后先在室温下反应1h,然后在60℃反应1h,反应液倾入700mL石油醚中析出产物,收率50%~60%. 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