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871.
Jiang Hu Wei‐Dong Zhang Yun‐Heng Shen Chuan Zhang Run‐Hui Liu Xi‐Ke Xu Bin Wang 《Helvetica chimica acta》2007,90(4):720-722
Two novel alkaloids, 4,5‐dihydroxy‐1‐methyl‐3‐oxo‐2‐(trichloromethyl)‐3H‐indolium chloride ( 1 ) and 4‐(2‐methoxyethyl)‐N,N‐dimethylbenzenamine ( 2 ), were isolated from the EtOH extract of the roots of Zanthoxylum nitidum. Their structures were identified on the basis of spectroscopic and mass‐spectrometric analyses. 相似文献
872.
873.
Ung-Ping Wang 《中国化学会会志》1973,20(2):57-73
Vinyl monomers such as vinyl acetate, vinyl chloride, methyl methacrylate and styrene etc., can be polymerized without catalyst into the composites of bagasse material by gamma-radiation induced in situ liquid polymerization process. The fundamental factors, such as polymerization-rate, effect of swelling agent, molecular weight of vinyl polymers and graft reaction between bagasse cellulose and vinyl polymers, have been investigated and discussed. The use of suitable low G-value polar swelling agents and the application of suitable gamma dose-rate are two key factors found to control the smooth in situ liquid polymerization system of vinyl monomers in bagasse. 相似文献
874.
Jinmao You Xiangming Chen Xianen Zhao Yourui Suo Honglun Wang Yulin Li Jing Sun 《Chromatographia》2006,63(7-8):337-343
A pre-column derivatization method for the sensitive determination of amines using the labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl
chloroformate (BCIC-Cl) followed by high-performance liquid chromatography with fluorescence detection has been developed.
Identification of derivatives is carried out by high performance liquid chromatography/atmospheric pressure chemical ionization
(LC-APCI-MS-MS). The chromophore of 2-(9-carbazole)-ethyl chloroformate (CEOC) reagent is replaced by 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl
functional group, which results in a sensitive fluorescence derivatizing reagent BCIC-Cl. BCIC-Cl can easily and quickly label
amines. Derivatives are stable enough to be efficiently analyzed by high-performance liquid chromatography and show an intense
protonated molecular ion corresponding m/z [MH]+ under APCI in positive-ion mode. The collision-induced dissociation of protonated molecular ion formed a product at m/z 260 corresponding to the cleavage of CH2-OCO bond. Studies on derivatization demonstrate excellent derivative yields over the pH 9.0–10.0. Maximal yields close to
100% are observed with a 3 to 4-fold molar reagent excess. In addition, the detection responses for BCIC derivatives are compared
with those obtained using CEOC and FMOC as derivatization reagents. The ratios of IBCIC/ICEOC and IBCIC/IFMOC are, respectively, 1.23–3.14 and 1.25–3.08 for fluorescent (FL) responses (here, I is relative fluorescence intensity). Separation of the derivatized amines had been optimized on reversed-phase Eclipse XDB-C8 column. Detection limits are calculated from 1.0 pmol injection, at a signal-to-noise ratio of 3, are 10.6–37.8 fmol. The
mean interday accuracy ranges from 94 to 105% for fluorescence detection with the largest mean %CV<7.5. The mean interday
precision for all standards is < 6.0% of the expected concentration. Excellent linear responses are observed with coefficients
of > 0.9997.
Revised: 12 December 2005 and 13 Febrauary 2006 相似文献
875.
Studies were made on oscillations across a liquid membrane consisting of an oil layer, octanol containing barbitone, between two aqueous layers: one containing 8 mM SDS with alcohol and the other containing 0.1 M NaCl. The effects of various concentrations of chemical components in this system on the patterns of electrical oscillation were examined. The oscillations may be explained by the mechanism of repetitive formation and destruction of monolayer structures of the dodecyl sulfate anion at the interface between the organic and the aqueous phases, with the effect of proton penetration. This study of potential oscillation across a membrane containing a drug provides the possibility of further investigations in pharmacological activity. 相似文献
876.
877.
878.
Fluoxetine (Prozac) is currently one of the widely prescribed selective serotonin reuptake inhibitors (SSRIs) for the treatment of depression. A high-throughput sample preparation procedure using liquid-liquid extraction (LLE) in a 96-well plate format in conjunction with liquid chromatography/tandem mass spectrometry (LC/MS/MS) was developed and validated for quantification of fluoxetine enantiomers in human plasma. After addition of internal standard and ammonium hydroxide, samples were extracted with ethyl acetate. The organic extract was evaporated to dryness and reconstituted in methanol. Where possible, sample transfer and LLE steps were automated using a Tomtec Quadra 96 workstation. Adequate separation of fluoxetine enantiomeric pairs (resolution of 1.17) was achieved on a vancomycin column eluted with methanol containing 0.075% (by weight) ammonium trifluoroacetate. A triple quadrupole mass spectrometer, operated in the multiple reaction monitoring mode at m/z 310-->44 for fluoxetine enantiomeric pairs and m/z 287-->241 for oxazepam (internal standard), was used. Analysis was performed in the positive ion mode using atmospheric pressure chemical ionization (APCI). The standard curve range was 2.0-1000 ng/mL for each fluoxetine enantiomer. The intra- and inter-day precision and accuracy of the quality control (QC) samples were <12.5% (CV) and <13.6% (CV), respectively, for each fluoxetine enantiomer; the correlation coefficient was >0.990. Method ruggedness was demonstrated by the reproducible performance of the assay during a three-day validation period. 相似文献
879.
负载型TiO2-聚酰亚胺亲水复合膜的制备与分离性能 总被引:4,自引:1,他引:4
采用溶解-流涎法,湿相转换法和干湿相转换法制轩了负载型TiO2-聚酰亚胺亲水复合膜,采用扫描电镜,红外光谱,压汞和透气性实验等手段对该膜的孔径分布,表面结构及扩散性能进行了表征,并讨论了制备亲水对膜孔结构的影响,实验结果表明,三种膜均具有很好的亲水性能,而干湿相转换膜具有良好的孔径分布和分离性能。 相似文献
880.
Wang D Schwinden MD Radesca L Patel B Kronenthal D Huang MH Nugent WA 《The Journal of organic chemistry》2004,69(5):1629-1633
The reaction of a variety of methyl esters with dimethylsulfoxonium methylide at 0-25 degrees C affords the chain-extended beta-keto dimethylsulfoxonium ylides. Subsequent treatment with hydrogen chloride in THF proceeds with loss of DMSO to afford the corresponding alpha-chloroketones. This sequence has been utilized to convert the methyl esters of CBZ-protected alanine and valine to the anti N-protected alpha-amino epoxides, which are important pharmaceutical intermediates. When the same protocol is applied to BOC-protected phenylalanine methyl ester, epimerization occurs so that the use of a more reactive aryl ester is required. This chemistry provides a practical route to alpha-chloroketones that avoids the use of toxic and explosive diazomethane. 相似文献