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11.
Gert Brandl Fritz Kastner Rainer Fritsch Herbert Zinner Albrecht Mannschreck 《Monatshefte für Chemie / Chemical Monthly》1992,123(11):1059-1069
Summary A procedure is described which serves to measure circular dichrograms () on line during stops of flow in liquid chromatography. Since the concentration of substrate in the spectrometer cell during the stop is not known, the differential absorption coefficients are calculated from the experimental differential absorbances A by means of UV absorption (i. e. photomultiplier voltage) data. Verifications of the procedure are obtained by its application to three substrates (Table 1), the () spectra of which were known. The present on-line technique is compared with a corresponding off-line method.The N,N-dimethylthiobenzamides1 and2 as well as the 9,10-phenanthrenequinone7 consist of interconvertible enantiomers because their planar states are destabilized by steric overcrowding of groups. The unknown dichrograms () of1, 2 and7 are obtained (Figs. 2 and 4) and discussed with reference to the helicities of these molecules.In memory of the late Professor Dr. Dr. h. c. Günther Snatzke. 相似文献
12.
Enantiomeric amide derivatives of (S)- and (R)-1-phenyl-2-aminopropane (dextro- and levoamphetamine, respectively) were resolved by high performance liquid chromatography on commercially available ionically and covalently bonded chiral stationary phases ((R)-N-(3,5-dinitrobenzoyl)phenylglycine). Ten enantiomeric amide pairs were synthesized and chromatographed on the columns by using a mobile phase of hexane-isopropanol (97 : 3), a flow rate of 2 ml/min, and a column temperature of 20°C. The (R)-isomer of all 10 amides eluted first on the covalent column as did the (R)-isomer of nine derivatives on the ionic column. however, the 3,5-dinitrobenzoyl amide of (S)- amphetamine eluted before the (R)-isomer on the ionic column. This reversal in enantiomeric elution order reveals the complexity of the interactions occurring on these columns and emphasizes the hazards of relying on observed elution order as an a priori indication of absolute configuration. 相似文献
13.
Summary The partial resolution of some drug enantiomers by counter-current extraction in an aqueous two-phase system using bovine serum albumin (BSA) or ovomucoid (OVM) as chiral discriminator is described. The phase system was prepared with dextran 40, polyethylene glycol and a protein. Ofloxacin (OFLX) enantiomer was well recognized by the BSA system, whereas the enantiomers of carvedilol (-blocker) and DG-5128 (a new oral hypoglycaemic drug) were hardly recognized by the OVM system. The distribution coefficients of (S)-, (R)- and rac-OFLX varied with pH. Good enantioselectivity for OFLX was obtained at relatively high pH ( pH 9). The crude optically enriched OFLX enantiomers were extracted from the aqueous fractions and finally purified by thin-layer chromatography. 相似文献
14.
Summary A new stationary phase [bikis(2,6-di-O-pentyl-3-O-hex-6-enyl)-pentakis(2,6-di-O-pentyl-3-O-methyl)-β-CD-polysiloxane] was
synthesized and successfully applied in GC for the separation of chiral and achiral isomers. It possesses high column efficiency
and exhibits excellent separation ability for disubstituted benzenes. Some typical enantiomers and optical isomers are well
separated. The separation behavior of this new phase is characterized and discussed. 相似文献
15.
Summary A new chiral ligand exchange selector for hydrophobic stationary phase modification has been synthesized by selective alkylation of L-histidine at the pyrrolic nitrogen atom in its imidazolic ring. Its performance was then tested on RP-HPTLC plates treated with copper acetate. Significant selectivity towards aromatic amino acid enantiomers, was observed. Chromatographic retention data were compared to available thermodynamic complex formation parameters for the relevant model systems in aqueous solution.Stationary and mobile phase effects on retention were studied by using different RP-HPTLC plates and various binary aqueous solvent mixtures.Optimized separation conditions for aromatic amino acid sample class are given. 相似文献
16.
Sergey?P.?BabailovEmail author Lubov?D.?Nikulina 《Journal of inclusion phenomena and macrocyclic chemistry》2005,51(1-2):103-109
1H and 13C NMR measurements are reported for the CDCl3 and CD2Cl2 solutions of [La(NO3)3(18-crown-6)] (I), [Pr(NO3)3(18-crown-6)] (II) and [Ce(NO3)3(18-crown-6)] (III) complexes. Temperature dependencies of the 1H NMR spectra of II have been analyzed using the dynamic NMR methods for multi-site exchange. Two types of conformational dynamic processes in II were identified (the first one with activation enthalpy ΔH
‡=26 ± 4 kJ/mol is conditioned by interconversion of complex enantiomeric form and pseudorotation of macrocycle molecule upon the C
2 symmetry axis, the second one with ΔH
‡=46 ± 5 kJ/mol is conditioned by macrocycle molecule inversion). Studies of the values of the lanthanide-induced shifts revealed that the structure of complexes in solution is similar to that reported for the complex I in the crystal state.This revised version was published online in July 2005 with a corrected issue number. 相似文献
17.
Summary Resolution of enantiomeric mixtures of DL-amino acids (Nine) using silica gel layers impregnated with (-)-bruncine is reported.
The solvent system used was Butanol: Acetic acid: Chloroform (3∶1∶4). The diastereomers were formed and hydrolysed, by dilute
HCl spray, on the chromatogram only and the amino acids thus resolved were located by ninhydrin spray. The cross resolution
possibilities of enantiomers were also calculated. 相似文献
18.
Ivan panik Jan Krupcik Ivan Skacani Jaap De Zeeuw Mario Galli Pat Sandra 《Journal of separation science》1997,20(12):688-692
The separation of isomers and enantiomers of branched C10-C12 phenylalkanes by gas chromatography on fused silica capillary columns coated with some modified β- and γ-cyclodextrins was studied. It was shown that the separation of positional isomers of C10-C12 phynylalkanes on modified cyclodextrin capillary columns is not better than that on a column coated with modified polyethylene glycol. Differences were found in the enantioselectivity of modified β- and γ-cyclodextrins for the separation of C10-C12 secondary phenylalkane enantiomers. While alkylderivatives of β-CDs resolve enantiomers of 3-phenylalkanes, alkyl derivatives of γ-CD resolve enantiomers of 2-phenylalkanes. Since shape selectivity factors of modified cyclodextrins have indicated no inclusion of the considered solutes in cyclodextrin cavities, enantioselective interactions most probably occur on the outer sphere of cyclodextrins. 相似文献
19.
以N,N-二甲基甲酰胺(DMF)为溶剂,丁酮为内标,采用PV-101毛细管色谱柱 (30 m×0.22 mm),氢火焰离子化检测器,建立兰索拉唑中五种有机溶剂甲醇、乙醇、丙酮、二氯甲烷、乙酸乙酯残留量的定量分析方法。五种有机溶剂检出限分别为0.002 4%,0.002 4%, 0.001 2%,0.000 6%,0.000 6%;在10-1000 mg·L-1浓度范围内,各组分线性关系良好;对应的平均回收率分别为100.8%±3.6%,102.1%±2.3%,99.97%±4.1%,99.63%±2.7%, 102.3%±3.5%。 相似文献
20.
Narayanan Balaji Bhavesh Babulal Gabani Umesh Todmal Suresh P. Sulochana Neeraj Kumar Saini Rajesh Chandran Ramesh Mullangi 《Biomedical chromatography : BMC》2019,33(3)
We developed and validated a simple, sensitive, selective and reliable LC–ESI‐MS/MS method for direct quantitation of dropropizine enantiomers namely levodropropizine (LDP) and dextrodropropizine (DDP) in rat plasma without the need for derivatization as per regulatory guidelines. Dropropizine enantiomers and carbamazepine (internal standard) were extracted from 50 μL rat plasma using ethyl acetate. LDP and DDP resolved with good baseline separation (Rs = 4.45) on a Chiralpak IG‐3 column. The mobile phase consisted of methanol with 0.05% diethylamine pumped at a flow rate of 0.5 mL/min. Detection and quantitation were done in multiple reaction monitoring mode following the transitions m/z 237 → 160 and 237 → 194 for dropropizine enantiomers and the internal standard, respectively, in the positive ionization mode. The proposed method provided accurate and reproducible results over the linearity range of 3.23–2022 ng/mL for each enantiomer. The intra‐ and inter‐day precisions were in the ranges of 3.38–13.6 and 5.11–13.8 for LDP and 4.19–11.8 and 8.89–10.1 for DDP. Both LDP and DDP were found to be stable under different stability conditions. The method was successfully used in a stereoselective pharmacokinetic study of dropropizine enantiomers in rats following oral administration of racemate dropropizine at 100 mg/kg. The pharmacokinetic results indicate that the disposition of dropropizine enantiomers is not stereoselective and chiral inversion does not occur in rats. 相似文献