国外MCM及其主要制造技术的发展现状

MCM具有胜过PCB、LSI和一般HIC的诸多优点,正在逢勃发展,可望成为九十年代的代表性技术。本文从市场和技术两个方面评述MCM的发展潜力,重点介绍近年来国外MCM主要制造技术的现状及发展态势,试图引起人们对它的关注。     

脂肪乳剂Intralipid代谢产物的高效液相色谱测定

本文介绍了利用ＨＰＬＣ色谱柱前衍生化技术简便，正确和灵敏地测定血清中游离脂肪酸的方法。在最佳条件下，一些脂肪酸的最低检知量为０．０４μｇ。方法已用于脂肪乳剂Ｉｎｔｒａｌｉｐｉｄ在诱发急性坏死性胰腺炎动物体内代谢产物测定。     

Immobilized polysiloxanes as stationary phases for high-performance liquid chromatography and solid phase extraction

Polysiloxanes immobilized onto the surfaces of porous silica particles have proven to be good stationary phases for the separation of multiresidues of pesticides and their metabolic/degradation products by reversed-phase high-performance liquid chromatography (RP-HPLC). Similar materials have proven effective for pre-concentration and clean-up procedures using solid phase extraction. The present paper describes the preparation and some applications of several of these packing materials.     

LC-MS/MS method for the confirmatory determination of aromatic amines and its application in textile analysis

A confirmation method for the determination of 18 aromatic amines originating from azo dyes after reductive cleavage was developed. The method is based on the use of high-performance liquid chromatography/tandem mass spectrometry with atmospheric-pressure chemical ionization. For the identification of the analytes one precursor ion and two daughter ions (multi-reaction monitoring, MRM) were selected and the LC-MS/MS parameters optimized to obtain high sensitivity and selectivity. The linear ranges varied from 0.1–1 to 30–50 g mL^–1 with correlation coefficients of 0.99 or better. The applicability of the method to determine o-tolidine (3,3-dimethylbenzidine) and 3,3-dimethoxybenzidine in textiles following reductive cleavage of acid red 114, trypan blue, and Chicago sky blue 6B was demonstrated.     

The application of chromatography to the analysis of pharmaceutical creams

Summary The application of GLC, HPLC and TLC to the analysis of pharmaceutical creams is discussed with special attention to sample clean-up. The results of the determination of hydrocortisone acetate, salicylic acid, benzoic acid, diethyl stilbestrol, chloramphenicol, diphenhydramine HCl, tretinoin and some cream base components by reversed phase HPLC are given.Presented at the 14th International Symposium on Chromatography London, September, 1982     

Donator-Acceptor Komplex Chromatographie Tetrachlorphthalimidopropylsilica,eine neue,chemisch gebundene Phase,geeignet zur Trennung von Kohleverflüssigungsprodukten und anderen technischen aromatischen Gemischen mit der Hochleistungsflüssigkeitschromatographie

Summary The preparation of a new tetrachlorophthalimidophase for HPLC is described. The capacity ratios (k) of about forty aromatics and twenty nitrogen-containing aromatics were determined. Most of the compounds used were alkylated. It was shown that the aromatics were eluted according to the number of rings, only slightly influenced by the substituents. A similar elution order was not observed with the heteroaromatics. The performance of the stationary phase is demonstrated, performing separations of coal liquids and other aromatic mixtures.

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Donator-Acceptor Komplex Chromatographie Tetrachlorphthalimidopropylsilica, eine neue, chemisch gebundene Phase, geeignet zur Trennung von Kohleverflüssigungsprodukten und anderen technischen aromatischen Gemischen mit der Hochleistungsflüssigkeitschromatographie

Zusammenfassung Es wird die Synthese einer neuen Tetrachlorphthalimid-Phase für die HPLC beschrieben. Anhand von Elutionsversuchen mit über vierzig Aromaten und zwanzig N-Heteroaromaten, die größtenteils alkyliert waren, konnte gezeigt werden, daß kondensierte Aromaten unabhängig vom Alkylierungsgrad streng nach der Zahl der aromatischen Ringe eluiert werden, was für die Heterocyclen nicht zutrifft. Die Kapazitätsverhältnisse (k) der untersuchten Verbindungen werden angegeben. Die Leistungsfähigkeit der Phase wird an der chromatographischen Trennung von Kohleverflüssigungsprodukten und anderen komplexen, aromatischen Gemischen demonstriert.

     

High-performance liquid chromatography of sulfonamides and quinolones on p-tert-butyl-calix[6]arene-bonded silica gel stationary phase

The high-performance liquid chromatographic behavior of some sulfonamides and quinolones was studied on a p-tert-butyl-calix[6]arene-bonded silica gel stationary phase. The effect of mobile phase variables such as methanol content, ionic strength and pH on their chromatographic behavior was investigated. The retention behavior of sulfonamides on the stationary phase was compared with that on both Zorbax C₁₈-bonded silica gel and γ-(ethylenediamino)propyltriethoxylsilane-bonded silica gel (diamino-bonded phase). The retention mechanism of sulfonamides and quinolones on the stationary phase was also discussed. The results indicate that the stationary phase behaves as a reversed-phase packing and its separation selectivity is much better than that of not only Zorbax C₁₈ phase but also diamino-bonded phase. Some sulfonamides and quinolones were separated on the stationary phase, but the separation of sulfonamides is far more successful.     

Determination of thiol by high-performance liquid chromatography and fluorescence detection with 5-methyl-(2-(<Emphasis Type="Italic">m</Emphasis>-iodoacetylaminophenyl)benzoxazole

A new high-performance liquid chromatographic (HPLC) method for measuring low molecular weight (LMW) thiol-containing compounds, including cysteine (CysH), glutathione (GSH), N-acetylcysteine (Nac), penicillamine (PA), and 2-mercaptoethanol (2-ME), has been developed by using 5-methyl-(2-(m-iodoacetylaminophenyl)benzoxazole (MIPBO) as fluorescence-labeling reagent. The derivatization and separation conditions have been investigated in detail. Detection limits ranging from 3.5 to 15.0 fmol were achieved for the thiols investigated in a 16 min separation with detection wavelengths 310 and 375 nm for the excitation and emission, respectively. The utility of the proposed method has been validated by measuring CysH in human urine samples.     

Fluorimetric assay for measuring Dns-His-Lys-Arg-His-Lys cleaving enzyme using high-performance liquid chromatography

A rapid and sensitive assay for the determination of Dns-His-Lys-Arg-His-Lys cleaving enzyme activity is reported. This assay is based on fluorimetric detection of a dansylated dipeptide, 5-dimethylaminonaphthalene-1-sulfonyl-His-Lys, enzymatically formed from the substrate 5-dimethylaminonaphthalene-1-sulfonyl-His-Lys-Arg-His-d-Lys, after separation by high-performance liquid chromatography (HPLC) using a C-18 reversed-phase column by isocratic elution. This assay is sensitive enough to measure 5-dimethylaminonaphthalene-1-sulfonyl-His-Lys at concentrations as low as 7 pmol, and yields highly reproducible results and requires less than 9.0 min per sample for separation and quantitation. The optimum pH for Dns-His-Lys-Arg-His-Lys cleaving enzyme activity was 7.5-8.0. The Michaelis constant (K_m) and the maximum velocity (V_max) values were 33.3 μM and 47.07 pmol/(μg h), respectively with the use of enzyme extract obtained from bovine pituitary. By using this assay, axonal transport of this enzyme activity was observed 48 h after double ligations of rat sciatic nerves. The high sensitivity and selectivity of this assay would be useful for clarification of the physiological role of this enzyme.