用毛细管电泳法对某些药物的分离试验

本文采用毛细管电泳法,以50μm内径,45cm长的弹性石英毛细管作为分离管,选用磷酸盐-硼酸盐-十二烷基硫酸钠缓冲溶液体系,在柱254nm紫外检测器,在不同的电泳电压下,对水溶性维生素,磺胺类药物、头孢菌素抗生素,解热镇痛药物有效成份进行了分析,取得较满意的结果。     

The effect of polyether terminal chains in the liquid crystalline behavior of ortho-palladated complexes

A series of benzylideneanilines bearing terminal polyether chains, HL (HL = R-C₆H₄-CHN-C₆H₄-R′: R = OC₈H₁₇, R′ = O(CH₂CH₂O)₂C₂H₅; R = O(CH₂CH₂O)₂C₂H₅, R′ = OC₈H₁₇; R = R′ = O(CH₂CH₂O)₂C₂H₅; R = OC₁₂H₂₅, R′ = O(CH₂CH₂O)₃C₂H₅; R = O(CH₂CH₂O)₃C₂H₅, R′ = OC₁₂H₂₅; R = R′ = O(CH₂CH₂O)₃C₂H₅) have been prepared. Their dinuclear, [Pd(μ-X)L]₂ (X = OAc, Cl, Br, SC₈), [Pd₂(μ-SCn)(μ-X)L₂] (X = OAc, Cl; n = 8, 2) and mononuclear orthopalladated derivatives, Pd(acac)L, Pd(Ala)L, are reported and their mesogenic properties are compared with those of the analogous compounds with alkoxy chains. In general a great lowering in the melting points is produced for all the products. The free ligands and the alanine complexes are not liquid crystals. The chloro-bridged complexes bearing alkoxy and short polyether chains (O(CH₂CH₂O)₂C₂H₅) show the larger improvement of mesogenic properties. Longer polyether chains (O(CH₂CH₂O)₃C₂H₅) result usually in a destabilization of the mesophases. If only polyether chains are present, the destabilization is important regardless of the chain length. The ability of these molecules as ionic extractants and transporters was qualitatively evaluated for the more propitious cis-dinuclear complexes, which in fact showed some extracting ability, modest but improved compared to the free ligands.     

Chiral recognition in the resolution of enantiomers by GLC

Summary Chiral recognition of many enantiomeric solutes by a chiral amide stationary phase is based mainly on hydrogen bonding. A chiral-recognition-factor CHI is proposed, given by the difference of the enthalpy change in the enantiomer discrimination, standardized with respect to the specific interaction of the solutes with the diamide core of the stationary phase. The r?le of the entropy part is also discussed. By extrapolation of the retention behaviour to elevated temperature, peak inversion of enantiomers is predicted. Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984     

Highly sensitive method for the determination of a new anthracycline: Pirarubicin

Summary A new and highly sensitive HPLC method for the simultaneous determination of pirarubicine (THP-doxorubicin) and its metabolites, adriamycin and adriamycinol, in human plasma, is described. Samples were treated by liquid-liquid extraction, the organic phase removed and the residue dissolved in methanol. Separation was on a Lichrocart Supersher RP 8 column, (250×4 mm) 4 m, with a mobile phase of acetonitrile/methanol/formate-buffer.     

穿过液膜的自发电势振荡

An artificial membrane consisting of pricramic acid in nitrobenzene was used as an oil phase imposed between two aqueous phases. The right one contained trimethyl-slearylammonium chloride and aicohol; and the left contained sucrose solution (or H_2O). We found that this system exhibited rhythmic oscillation of electrical potential. The amplitude of the oscillations was between 20—150 mV. The oscillations were observed even when ethyl alcohol was absent in the aqueous of trimethylslearylammonium Chloride, and the increase in amplitude of oscillation with time was found to be less in the presence of sucrose. Some of the expremental results have been explained.     

维生素B类药物在薄层原位的近红外付立叶变换表面增强拉曼光谱

维生素Ｂ类药物在薄层原位的近红外付立叶变换表面增强拉曼光谱汪瑗，于秉正张煦（首都师范大学分析测试中心北京１０００３７）（北京大学分析测试中心北京）关键词维生素Ｂ_１，维生素Ｂ_２，薄层色谱，表面增强拉曼散射，近红外付立叶变换拉曼光谱将薄层色谱（ＴＬＣ）...     

Trace anion determination in concentrated hydrofluoric acid solutions by two-dimensional ion chromatography I. Matrix elimination by ion-exclusion chromatography

Since years, ion exclusion chromatography (ICE) has been the standard method to separate strong acid analyte anions from concentrated weak acid matrices such as hydrofluoric acid (HF). In this work, the commercially available IonPac ICE-AS 1 column was used to separate trace levels of chloride, nitrate, sulfate and phosphate from HF solutions at 20% (w/w). The efficiency of the separation was studied in more detail using techniques such as ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP-OES) and ICP-mass spectrometry (ICP-MS). For 20% (w/w) HF solutions and at a water carrier flow-rate of 0.50 ml/min, the cut window was set from 8.5 to 14.5 min. Under these conditions, analyte recoveries of better than 90% were obtained for chloride, nitrate and sulfate, but only about 75% for phosphate. The HF rejection efficiency was better than 99.9%. It was found that the ICP techniques, measuring total element levels and not species, yielded significantly higher recoveries for phosphorus and sulfur compared to IC. Evidence will be given that part of the added phosphorus (approximately 15% for an addition of 10 mg PO4/kg) is present as mono-fluorophosphoric acid (H2FPO3). In the case of sulfate, the difference between IC and ICP-MS could be attributed to an important matrix effect from the residual HF concentration.