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141.
Deng C Li N Wang X Zhang X Zeng J 《Rapid communications in mass spectrometry : RCM》2005,19(5):647-653
In the current work, a simple, rapid, accurate and inexpensive method was developed for the determination of acetone in human blood. The proposed method is based on derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA), followed by headspace liquid-phase microextraction (HS-LPME) and gas chromatography/mass spectrometry (GC/MS). In the present method, acetone in blood samples was derivatized with PFBHA and acetone oxime formed in several seconds. The formed oxime was enriched by HS-LPME using the organic solvent film (OSF) formed in a microsyringe barrel as extraction interface. Finally, the enriched oxime was analyzed by GC/MS in electron ionization (EI) mode. HS-LPME parameters including solvent, syringe plunger withdrawal rate, sampling volume, and extraction cycle were optimized and the method reproducibility, linearity, recovery and detection limit were studied. The proposed method was applied to determination of acetone in diabetes blood and normal blood. It has been shown that derivatization with HS-LPME and GC/MS is an alternative method for determination of the diabetes biomarker, acetone, in blood samples. 相似文献
142.
本文研究了Cu(Ⅱ)-PEG(聚乙二醇-2000)-Zincon(锌试剂)-(NH4)2SO4体系的析相光度法并应用于测定Cu(Ⅱ)。最宜酸度为pH5.5~8.5(KH2PO4-K2HPO4)缓冲溶液)其络合物的最大吸收位于610nm,表观摩尔吸光系数为4.0×10^4L.mol^-1.cm^-1,Cu(Ⅱ)浓度在0~1.5mg/L范围内服从比尔定律,铜与Zincon形式组成为1:2的稳定的蓝色络 相似文献
143.
An oligosaccharide homologue named SnS-2 was isolated from the root of Scrophularia ningpoensis Hemsl.SnS-2 was purified by means of gel-permeation chromatography and ion-exchange chromatography. Its physicochemical properties, including carbohydrate content and molecular weight were determined. The structure of SnS-2 was elucidated by chemical methods along with ^1H and ^13C NMR spectroscopy, including two-dimensional DQCOSY and H-detected ^1H, ^13C HMQC experiments. These results show that SnS-2 possesses a backbone consisting of terminal α-Galp-(1→, α-Galp-(1→6), α-Glcp-(1→6) and nonreducing end β-Fruf-(2→. The bioactive assay showed that it could inhibit the growth of Lewis pulmonary carcinoma implanted in mice. 相似文献
144.
压力流驱动电色谱分析方法及其若干色谱行为 总被引:1,自引:0,他引:1
压力流驱动电色谱分析方法是一种新型色谱技术。它组合了HPLC和电泳两种技术,为分离提供了更多可控制的因素。介绍了压力流驱动电色谱的装置和毛细管电色谱柱的装置方法,从理论上讨论了影响电色谱分离的因素并用实验数据加以证明。最后尝试性地将电色谱法用于测定香蕉样品中萨索啉(Salsolinol)等的含量。 相似文献
145.
Yong Deng Da Cheng Yang Yi Shen Yu Guo Zhong 《中国化学快报》2007,18(1):7-9
Based on the structure-activity relationships and antiangiogenic mechanism of RGD-containing peptides,a series of 5-amino- 1,3-dihydro-1,3-dioxo-2H-isoindole derivatives were synthesized.The structures were characterized by ~1H NMR,MS and elementary analysis.There ability to inhibit angiogenesis were evaluated by chick embryo chorioallantoic membrane assay at 10~(-5) mol/L.Compounds 7a and 7b displayed obvious antiangiogenic activity. 相似文献
146.
147.
研究了高效液相色谱-火焰原子吸收光谱联用系统分析信号处理方法,比较了各种处理方法的优缺点,用积分与适应平滑法综合处理色谱峰分析信号,不仅能有效地消除噪声,而且能使分析信号得到加强,以测定镍为例,经积分与适应平滑法综合处理后,检出限改善了2.7倍。 相似文献
148.
Xu‐Cheng Fu Xiao‐Yan Wang Ming‐Tian Li Xiao‐Tao Deng Cheng‐Gang Wang 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(8):m343-m345
The title complex, {[Cu2(C8H4O4)2(C3H4N2)4(H2O)]·H2O}n, is a three‐dimensional polymer formed through bridging by phthalate dianions of two different CuII cations and a network of O(N)—H⋯O hydrogen bonds. The Cu—O and Cu—N interaction distances are in the ranges 2.0020 (16)–2.4835 (17) and 1.968 (2)–1.9855 (19) Å, respectively. The structure is composed of alternating polymer chains parallel to the c axis, with a shortest Cu⋯Cu distance of 6.3000 (5) Å. 相似文献
149.
Using the mixture of cetyltrimethylammonium bromide (CTAB) and p‐Octyl polyethylene glycol phenyl ether (OP‐10) as templates, siliceous MCM‐48 materials can be synthesized with low molar ratio of CTAB to silica (0.139:1) and low concentration of mixed surfactants (ca.5%) and within a wide range of OP‐10/CTAB ratio (0.08?0.25). The materials were characterized by X‐ray powder diffraction, N2 adsorption/desorption isotherm, TEM, TG‐DSC and 29Si MAS NMR. Measurements indicated that the use of mixed surfactants allowed better condensation and higher ordering of the cubic mesostructure; at the same time, some properties of these materials were sensitive to the OP‐10/CTAB ratio. It was also found that the reduced pH of the gel which had been crystallized for a certain time gave a highly reproducible synthesis with a high silica yield (about 95%). Furthermore, the reaction mechanism of the synthesis is discussed in detail. 相似文献
150.
磷酸铝类分子筛是近年来继Y型和ZSM七分子筛之后的第三代合成分子筛材料,其骨架由A10。和P0。四面体均匀交替地组成问.由于带负电行的A10。和带正电荷的PO。四面体数目相等,整个骨架呈电中性,所以这类分子筛本身无离子交换能力和催化活性.当用硅或某些金属离子(如Mg、Fe、Co、Zn等)对磷酸铝分子筛进行同晶取代,就会在骨架上造成电行不平衡,从而使这类分子筛具有一定的离子交换能力和酸性【习.因而对硅或金属离子在磷酸错类分子筛中取代机理的研究一直是人们感兴趣的问题问.Vpl-5是最近才合成出来的具有18圆环一维孔结构的… 相似文献