手性药物分析方法研究进展

综述了近10 年来手性药物分离检测方法的发展,包括高效液相色谱法、气相色谱法、毛细管电泳法,以及超临界流体色谱法等,旨在为该领域的进一步发展提供参考。     

气相色谱法检测腹部厌氧菌感染

本文就40例腹部感染标本进行气相色谱法检测厌氧菌,并与培养法对照。结果证明,临床标本直接用气相色谱法检测,与常规培养法比较,有速度快、精确度高、不受药物及细菌死亡的影响,标本用量少等优点,该法有临床实用价值。     

氨基酸分析检测方法的研究进展

对氨基酸分析常用的检测方法:分光光度法、气相色谱法、液相色谱法、毛细管电泳法及其它方法(近红外光谱法、化学发光法、荧光光谱法)进行综述,并介绍了这些方法在氨基酸检测中的应用,为建立快速、高效的氨基酸分析方法提供参考.     

薄层色谱法分离植物种子中主要不饱和脂肪酸的研究

测定植物种子中主要不饱和脂肪酸,在油脂品质鉴定、营养研究、油料作物品种选育(特别是油菜)以及发掘新的有价值的油料植物资源等方面,都有重要意义。现在检测菜籽油芥酸含量的方法有:气相色谱法、纸色谱法、冷冻法、分步沉淀法和混浊法。用于分离较长链不饱和脂肪酸的方法除了气相色谱     

高效液相色谱法测定月饼中的苯甲酸

关于月饼的苯甲酸检测没有明确的处理和检测方法,按照国标GB/T5009.29-2008的要求第一法气相色谱法和第二法液相色谱法进行检测。气相色谱法前处理涉及有机溶剂的重复萃取,操作时间较长,比较麻烦,液相色谱法也没有明确月饼的前处理方法。本文结合液相色谱法中的试样处理中的方法,对月饼的检测,采用了样品粉碎均匀称样后90度水浴30分钟的方法,加蛋白质沉淀剂定容过滤后直接进样,缩短了检测的时间,提高了工作的效率,适合大批量处理样品。     

气相色谱法测定结核菌耐药性的研究

本文应用气相色谱法对结核菌的耐药性进行了研究。在与传统法对比试验中,两法符合率为86.4%。气相色谱法可在6天报告比较准确的结果,比传统试管法提前2周,提示此法有较大的实用价值。     

银耳多糖单糖组成分析的三种色谱方法比较

为选择一种准确快捷的方法测定银耳多糖的单糖组成,对薄层色谱法(TLC)、气相色谱法(GC)、高效液相色谱法(HPLC)三种色谱方法进行比较。结果表明,前两种方法的测定结果均不理想,而HPLC法,操作简便,灵敏度高,分离效果好,信息完整。测定结果为由葡萄糖、甘露糖、葡萄糖醛酸、木糖、岩藻糖组成,其摩尔比为0.24∶1.00∶0.06∶0.29∶0.25。HPLC法对酸性杂多糖组成糖分析是一种比较理想的选择。     

L-肉碱的检测方法

Ｌ 肉碱是参与生物体新陈代谢的重要物质,本文简要介绍和比较了检测肉碱的７种主要方法,即生物法、化学法、酶法、荧光法、高压液相色谱法、 Ｎ Ｍ Ｒ和放射酶法,其中以酶法、荧光法和高压液相色谱法较为常用。     

有机磷农药检测方法研究进展

本文综述了当前国内外对于有机磷农药残留的几种主要检测分析方法,主要有色谱法、波谱法、免疫法等。并分析了各种检测方法的特点。     

发酵液中丁二酸的分析

分析与其它二元酸混杂着的丁二酸时,多用气相色谱法。但该法必须先除去其它杂质,然后经过定量酯化才能进行分析,操作颇繁杂。近年采用液体色谱法,较为方便。但该法所需仪器目前尚未普及。我们在工作中设计了不必先分离掉反丁烯二酸,α-酮戊二酸和苹果酸     

Application of centrifugal force to the extraction and separation of parasorboside and gerberin from Gerbera hybrida

A method for the separation of parasorboside and gerberin from the ornamental plant Gerbera hybrida (Asteraceae) has been developed. The two closely related glucosides were extracted using an Extrachrom instrument, a prototype multi-functional separation tool equipped with an extraction chamber. The rotation planar extraction procedure was compared with that of a medium pressure solid-liquid extraction system. The resulting extracts were pre-purified using rotation planar chromatography and the results compared with those obtained using medium pressure liquid chromatography with silica gel as the stationary phase and a mobile phase of methanol:ethyl acetate:tetrahydrofuran at selectivity point Ps = 111 with 1% formic acid as modifier. The title compounds were isolated from the purified extracts by TLC and their structures confirmed by 1H- and 13C-NMR spectroscopy.     

Simultaneous analyses of phenethylamine, phenylethanolamine, tyramine and octopamine in rat brain using fluorescamine

A fluorometric method for the simultaneous analyses of phenethylamine, phenylethanolamine, tyramine and octopamine has been developed. The method involves ion-exchange chromatography, derivatization with fluorescamine, solvent extraction and then separation by thin-layer chromatography. The fluorescent spots are then quantitated by scanning. The detection limits of this method are about 10 pmoles for phenethylamine, phenylethanolamine and tyramine, and 20 pmoles for octopamine. The method was used for simultaneous analyses of putative neurotransmitter amines in whole rat brain.     

Size exclusion chromatography for extraction of serum bile acids

A major problem in the measurement of serum bile acids is their quantitative extraction from the high molecular protein matrix. In our hands, the standard techniques of adsorption and reversed-phase chromatography have yielded incomplete recovery for different bile acids (33-93%) and poor reproducibility. In contrast, with the novel extraction procedure of size exclusion chromatography, recovery was nearly quantitative (75-104%) and reproducibility was satisfactory. The described method allowed for a reliable determination of serum bile acids in healthy subjects and patients with liver cirrhosis. We conclude that size exclusion chromatography for serum bile acid extraction is more reliable than alternative techniques, because the separation by size is independent of solubility, charge, and polarity.     

Gas chromatographic determination of free amino acids and amino acids attached to transfer RNA in biological samples

A method was developed to analyze quantitatively free amino acids and amino acids attached to transfer RNA (tRNA) in tissue samples by gas chromatography. Free amino acids were purified by ion-exchange chromatography after deproteinization. Total cellular aminoacyl-tRNA was extracted from rabbit reticulocytes and liver by a modified phenol extraction method under conditions which were designed to prevent deacylation of the attached amino acids. After deacylation and separation from tRNA by pressure ultrafiltration, eighteen amino acids were determined by gas chromatography as their N-heptafluorobutyryl isobutyl derivatives.     

Analysis of 3-indolylacetic acid and abscisic acid by high-performance liquid chromatography and gas-liquid chromatography

A method of analysis of 3-indolylacetic acid (IAA) and abscisic acid (ABA), allowing the simultaneous extraction of both regulators from plant material, has been developed. The method involves extraction with methanol, isolation of the acid fraction, diazomethane methylation, separation of the hormones through reverse-phase preparative high-performance liquid chromatography, and quantification of both compounds by gas-liquid chromatography. The recovery percentage at each step was monitored with radioactive compounds added at the beginning of the process. The final recovery was 70% for IAA and 96% for ABA. The method was applied to the analysis of the IAA and ABA content of stems of hazel (Corylus avellana L.).     

Fast, fully automated analysis of voriconazole from serum by LC-LC-ESI-MS-MS with parallel column-switching technique

Voriconazole is a novel broad-spectrum antifungal agent. We developed an on-line LC-LC-MS-MS method for fully automated and direct analysis of voriconazole in raw human serum. After injection of human serum size-selective sample fractionation and analyte extraction was achieved using an extraction column (25 mm x 4 mm) packed with a restricted access material (RAM, LiChrospher ADS C(8), 25 microm). On-line transfer of voriconazole from the extraction column was followed by chromatography separation on a C(18) column. Detection was done by ESI-MS-MS. The total analysis time was 13 min, managed by parallel extraction and chromatographic separation. This LC-MS assay was fully validated. The lower limit of quantification was 0.05 microg/ml. The automated inline extraction of voriconazole described here eliminates the need for difficult and time-consuming sample pre-treatment. Other advantages of the new method are that only a small quantity (5 microl) of serum is needed and that the method is very specific.     

Acyl-coenzyme A: cholesterol acyltransferase assay: silica gel column separation of reaction products

Acyl-coenzyme A:cholesterol acyltransferase (ACAT) assays are usually performed by incubation of the enzyme with a labeled substrate followed by thin-layer chromatography separation and subsequent quantification of cholesteryl esters (CE) formed. Herein, a method is described for rapid separation of CE from other lipids, by elution from a silica gel column with a solvent mixture of petroleum ether/diethyl ether (98:2, v/v). Silica gel column chromatography is reliable and more rapid and safer than TLC. The best results were obtained when the reaction was stopped by Dole extraction followed by CE separation on a silica gel column. Assays for ACAT from rat intestinal microsomes showed that the specific activity values obtained using this method were reproducible and in good agreement with those obtained by conventional TLC method.     

现代生物工程分离提取技术在海洋生物资源开发上的应用

本文综述了在海洋资源开发上应用的现代生物工程分离技术。介绍了最新的分离提取技术如制备型和生产型色谱技术、超临界萃取技术、膜分离技术、毛细管电泳技术、酶工程技术等。从海洋生物资源中提取有用的生物活性物质,需要符合特定要求的现代生物工程技术。其中柱层析技术和超临界萃取技术是海洋生物活性物质分离提取技术中的主要部分。     

A simple rapid method for ganglioside isolation from small amounts of tissue.

Gangliosides from as little as 1 mg dry wt of brain tissue can be isolated for thin-layer chromatography by a simple, rapid method which combines extraction by chloroformmethanol with a single step silicic acid column separation of gangliosides from the bulk of nonganglioside lipids.     

Concentrated,digestible DNA after hydroxylapatite chromatography with cetylpyridinium bromide precipitation

A method for the direct extraction of the DNA from the unfavorable phosphate eluant of hydroxylapatite chromatography is described. The DNA—reversibly precipitated with the cationic detergent cetylpyridinium bromide—can be subjected to further enzymatic manipulations within minutes. This method is applied to the rapid separation of pBR322 plasmid from the chromosomal DNA.