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毛细管气相色谱法对大麻中主要成分的定性定量分析 总被引:6,自引:0,他引:6
采用毛细管气相色谱法测定大麻中大麻酚、四氢大麻酚和大麻二酚的含量。以氯仿为提取溶剂,甲醇为色谱溶剂,用HP-5(10m×0.53mm×2.65μm)柱,以柱温220℃进行测定。大麻二酚、四氢大麻酚和大麻酚在20~120mg/L的浓度范围内线性关系良好,r分别为0.9994,0.9991和0.9995,回收率分别为97.3%~104.0%,97.3%~106.6%和95.3%~102.4%,最低检测限均为0.2μg/mL。利用3种主要成分保留时间的良好重现性也可进行定性。方法简便、快速、准确、灵敏。 相似文献
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高效液相色谱法测定低聚果糖的组分 总被引:9,自引:1,他引:8
采用高效液相色谱法(HPLC),以μ-BondapakC18柱为分析柱,水为流动相,示差折光仪为检测器,一次进样能同时测定低聚果糖样品中的果糖、蔗糖、三糖、四糖、五糖、六糖等。测定了“博爱生命素”样品,所得结果良好,变异系数为0.55%~1.1%,线性相关系数为0.9992~1.000。低聚果糖的最低检出限在微克级。 相似文献
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柱后衍生高效液相色谱法测定鸡肉中莫能菌素残留量 总被引:7,自引:0,他引:7
样品用甲醇-水溶液匀浆、提取后过滤,再用二氯甲烷进行液-液萃取,然后通过Sep-Pak柱进一步净化。净化后的样液与香兰素衍生试剂在酸性和加热条件下进行柱后衍生,反应产物在520nm波长处测定。衍生剂:香兰素30.0g+浓硫酸20mL+甲醇950mL,流速:0.7mL/min;色谱柱:μ-BondapakTMC183.9mmi.d.×300mm,或相当的色谱柱;流动相:V(甲醇)V(水)V(磷酸)=940601,流速0.7mL/min;柱后反应室:体积大于1.4mL的不锈钢管(300cm×1mmi.d.)。 相似文献
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提出了一系列的安全、方便、可靠、在线和可连续操作的热解吸/色谱分析柱制备S2OF10纯品、指数稀释法配制S2OF10标准样品、应用定量校正系数测定样品中痕量S2OF10的方法和技术。分别采用气相色谱、红外光谱、气相色谱/质谱等方法对色谱制备的S2OF10纯品进行了纯度分析和测定。配制S2OF10标准气体的体积分数范围为8.0×10-7~2.6×10-4。气相色谱测定S2OF10的定量校正系数为0.197,测定方法的相对误差范围为1.8%~20%。 相似文献
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PIA活性碳纤维在线富集水样中痕量元素及ICP—AES检测 总被引:3,自引:0,他引:3
本文研究了新型吸附材料-活性碳纤维的在线分离富集特性,用FI活性碳纤维填充的锥形柱,实现痕量金属元素Zn、Pb、Ni、Co、Cd、Mn的在线富集。经HNO3洗脱后,由ICPAES检测,测定速率达30样/h,检出限(ng/mL)分别为:0.4(Zn)、4.0(Pb),0.9(Ni)、0.4(Co)、0.4(Cd)、0.7(Mn),富集柱可使用多次。 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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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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《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