Determination of Amino Acids by High-Performance Liquid Chromatography with Electrochemical Detection Using Ferrocene Derivatization Reagents

Abstract

Two new reagents possessing ferrocene as an electrophore and isothiocyanate reactive toward the amino group were prepared and evaluated for pre-column derivatization of amino acids in high-performance liquid chromatography with electrochemical detection. The utilities of these reagents were investigated employing glycine as a model compound. Ferrocenylisothiocyanate was more favorable with respect to reactivity and electrochemical properties. The newly developed method was applied to the determination of 4-aminobutyric acid in biological specimens.     

Determination of Fatty Acids by High-Performance Liquid Chromatography with Electrochemical Detection Using A Ferrocene Derivatization Reagent

Abstract

New derivatization method using ferrocene reagents has been developed for the determination of fatty acids by high-performance liquid chromatography with electrochemical detection. Condensation of fatty acids with 3-bromoacetyl-1, 1'-dimethyl-ferrocene was effected in the presence of 18-crown-6 and potassium fluoride. The resulting esters showed the satisfactory sensitivity at +0.60 V vs. an Ag/AgCl reference electrode with a detection limit of 0.5 pmole. Also the high selectivity was obtained by using a twin electrode electrochemical detector. The proposed derivatization method was found applicable to the determination of fatty acids in human serum.     

Derivatization of Ketosteroids for High-Performance Liquid Chromatography with Electrochemical Detection

Abstract

A highly sensitive and selective derivatization of ketosteroids for use in high-performance liquid chromatography with electrochemical detection (HPLC/EC) is described. When the detector response for three phenylhydrazone derivatives was compared with one another using dehydroepiandrosterone, the p-nitrophenylhydrazone showed the highest sensitivity with a detection limit of 200 pg. Dehydroepiandrosterone and other principal 17-ketosteroids in human blood were quantitatively derivatized into p-nitrophenylhydrazones and efficiently separated by HPLC/EC on a μBondapak C_{1 8} column using 0.5%. NH₄H₂PO₄/methanol (2:7, v/v).     

液相色谱-电化学衍生-光学检测技术研究进展

综述了以反相键合相为主的高效液相色谱-柱后电化学衍生-荧光检测(RP-HPLC/ED/FD)技术的研究进展。对RP-HPLC/ED/FD存在的主要问题进行了讨论。并介绍了离子色谱-柱后电化学衍生-光学联用装置的构建及其在极性有机物和金属离子的测定方面的应用研究。     

Determination of Sulfophenyl Carboxylic Acids in Agricultural Groundwater Samples by Liquid Chromatography with Fluorescence Detection

Abstract

We have developed an analytical method to determine six sulfophenyl carboxylic acids (SPC) in agricultural groundwater samples. It involves a solid-phase extraction (SPE) procedure and subsequent separation and determination using liquid chromatography with fluorescence detection (LC–FD).The quantification limits ranged between 0.7 and 1.2 ng ml^?1. The proposed method was proved satisfactorily for the detection and determination of these compounds in groundwater samples during a study into the biodegradation of linear alkylbenzene sulfonates (LAS) in an agricultural soil sampled from the irrigated plain to the west of Granada (Spain).     

高效液相色谱法对手性药物罗格列酮与吡格列酮的拆分

采用高效液相色谱法,在多糖类手性固定相Chiralpak IC上成功拆分了2种降糖类手性药物罗格列酮与吡格列酮,考察了流动相、流速、温度、酸碱添加剂等对手性分离的影响.以正己烷-异丙醇(70:30,体积比)为流动相,在流速1.0 mL/min、检测波长254 nm、柱温35 ℃的条件下,罗格列酮与吡格列酮均得到良好分离,选择因子(α)分别为1.29、1.22,分离度(Rs)分别为7.07、5.56;该法不仅适用于此类手性药物的生产及质量控制,同时还可应用于对映体制备.     

N-羟基琥珀酰亚胺-3-吲哚乙酸酯柱前衍生高效液相色谱分离及荧光测定肽及其水解物

本文首次报道了一种新的羧酸活性酯试剂,N-羟基琥珀酰亚胺-3-吲哚乙酸酯作为柱前荧光衍生试剂,流动相为10mmol/L柠檬酸-Na₂HPO₄－pH 3.6的甲醇/水(20/80,V/V)溶液,C₁₈柱,于λ_cx/λ_cm＝278nm/355nm处进行荧光检测,高效液相色谱分离测定了谷胱甘肽、二甘肽、谷氨酸、胱氨酸、甘氨酸.当S/N＝3时,检出限为0.2至2.5Pmol.     

Liquid Chromatography Detertmination of Amino Acids by Pre-Column Fluorescence Derivatization with Acridone-N-acetyl Chloride

AminoacidsareimPortantconstituentSofmostlivingorganisms.Separationsandquantitativedetendnationsofandnoacidsbymeansofnewfluorescencereagentsforpre-columnorpost-columnderivatizationinRI,-HPLCarestillanactivefiled.InformationonderivahzationtechniquesforaminocomPoundshasbeencompiledbyBlanlandbyKnaPP'.Severalfluorescentderivatizationreagents'-'havebeendevelopedforthedeterminationofaminocomPounds.oPAmethodoffersgreatersensitivity,butisonIylimitedtoprimaryandnoacids.PIB-ClmethodisnotaPpropri…     

直接电导检测-离子排斥色谱法测定芳香族羧酸

研究了直接电导检测-离子排斥色谱法分离测定芳香族羧酸(邻苯二甲酸、水杨酸、苯乙酸、对羟基苯甲酸、苯甲酸和邻甲苯甲酸)。以Shim-packSCR-102H色谱柱为分离柱,H2SO4为流动相,考察了流动相浓度、色谱柱温度、流速对分离和测定芳香族羧酸的影响,确定最佳色谱条件为:0.08mmol/LH2SO4作为流动相,柱温45℃,流速1.2mL/min。所测芳香族羧酸的检出限为0.07～0.98mg/L;相对标准偏差在2.6%以下(n=5);回收率为95.8%～100.1%。本方法用于酱油样品的分析,得到满意结果。     

高效液相色谱化学发光检测法测定氨基酸

本文根据铜与氨基酸组成的１：１不饱和络合物对Ｌｕｍｉｎｏｌ－Ｈ２Ｏ２化学发光体系的催化活性，设计了一种新型氨基酸高效液相色谱化学发光检测器，即在色谱柱后安装一个氢氧化铜柱，从柱后流出的氨基酸通过氢氧化铜柱时，产生配合溶解形成氨基酸－铜（１：１）络合物，进行化学发光检测，１４种常见氨基酸的检测限均在ｐｍｏｌ级，已用于血清、尿和啤酒中氨基酸的测定。     

金属配位剂衍生-高效液相色谱法测定粮食及白酒中的游离氰化物

采用金属配位剂Ni(Ⅱ)-NH3作为衍生剂,与游离氰化物反应生成稳定且具有高紫外吸收值的Ni(CN)_4~(2-),使用高效液相色谱-紫外检测法(HPLC-UV)检测游离氰化物.方法的线性范围为0.014～0.540 mg/L,相关系数R~2=0.9984,检出限为4.0 μg/L.该方法简便快速,抗干扰能力强,灵敏度高,适于食品、环境、生物等样品中游离氰化物的检测.     

化学衍生-高效液相色谱法测定硫氰酸根阴离子

以α-溴-2,3,4,5,6-五氟甲苯作柱前衍生试剂,经优化衍生和色谱条件,实现了用高效液相色谱法测定硫氰酸根离子。在ODS柱上,用甲醇-水(80:20)作流动相,于254nm检测,得到线性关系良好的工作曲线,最小检测限为4.7ng。分析了吸烟者唾液样品,回收率为93.7％～101.4％。     

以邻苯二甲醛与N-乙酰-L-半胱氨酸作为柱前手性衍生化试剂拆分 DL-氨基酸的反相高效液相色谱法研究

本文用邻苯二甲醛和N-乙酰-L-半胱氨酸作柱前手性衍生化试剂,经反相高效液相色谱法拆分DL-氨基酸。研究了衍生化反应条件以及固定相、流动相对出峰顺序和分离效果的影响。实现了11对DL-氨基酸的同时拆分。本方法用于(±)-2,4,6三甲基苯丙氨酸的分离取得满意结果。     

In-Block Derivatization of Herbicidal Carboxylic Acids by Pentafluorobenzyl Bromide

Abstract

Herbicidal carboxylic acids were analyzed via ECD gas chromatography of their pentafluorobenzyl esters. The derivatives were formed by direct injection of a mixture of the acids and pentafluorobenzyl bromide in acetone; yields showed marked dependence on pKa of the acids. Carboxylic acids which have pKa values greater than 4.5 yielded the corresponding derivatives in poor yield unless triethylamine is included in the mixture. The procedure is fast and particularly convenient for low-level screening, identification and analysis of highly acidic chlorobenzoic, chlorophenoxyalkanoic, and arylacetic acids in the presence of less acidic carboxylic acids and phenols.     

间接液相色谱电化学法测定酯类化合物

本文用间接液相色谱电化学的方法对非电活性的酯类混合物甲酸甲酯、甲酸乙酯、乙酸甲酯和乙酸乙酯进行了分离和测定,其线性范围分别是3.2×10~(-9)～4.4×10~(-8)mol、2.4×10~(-9)～2.8×10~(-8)mol、2.0×10~(-9)～4.0×10~(-8)mol和2.2×10~(-9)～2.4×10~(-8)mol。对甲酸甲酯8次平行测定的相对标准偏差为0.89％。     

高效液相色谱荧光衍生法检测醇和酸的进展

高效液相色谱荧光衍生化醇和酸能提高检测灵敏度,改善分离效果,综述了最近十多年来高效液相色谱荧光衍生法检测醇和酸的进展情况。列出了衍生化试剂的结构,评述了衍生化的反应条件。指出了今后的发展方向。     

Nitroaromatic Reagents for Determination of Amines and Amino Acids by Liquid Chromatography/Electrochemistry

Abstract

Trinitrobenzene sulfonic acid, 2,4-dinitrofluorobenzene and 2-chloro-3,5-dinitropyridine were compared in terms of properties relevant to use as precolumn derivatization labels for amino compounds. This included consideration of chemical characteristics as well as purely detector oriented behavior. Trinitrobenzene sulfonic acid appears to be superior in all respects, yielding the most detectable derivatives with minimum production of interfering by-products.     

柱前衍生高效液相色谱法测定食物中氨基酸含量

采用柱前衍生高效液相色谱法,测定了食物中天冬氨酸、赖氨酸、亮氨酸等１６种氨基酸含量。衍生试剂为６－氨基喹啉基－Ｎ－羟基玻珀酰亚氨基甲酸酯（ＡＱＣ）,流动相为磷酸盐与峰面积呈良好的线性关系,相关系数均在０．９９以上,回收率在８８％～１１０％之间,样品测定结果良好。     

新型衍生试剂柱前衍生氨基酸的高效液相色谱分析

以邻硝基苯磺酰氯为标记试剂,RP-HPLC为分析模式,建立了一种新的氨基酸衍生化方法.通过液质联用对产物进行定性,研究并确定了最佳衍生化条件:衍生温度25 ℃,缓冲液pH9.0,衍生时间10 min.实验建立了20种氨基酸的HPLC分离方法:选用Kromasil C18柱,流动相A为30 mmol/L的NH4Ac溶液(pH 7.5),B相为乙腈;采用梯度洗脱,检测波长275 nm,室温.20种氨基酸在0.025 ～6.4 mmol/L范围内线性关系良好,相关系数在0.998 0 ～0.999 8之间,检出限为0.01 ～0.113 nmol.     

直接衍生/高效液相色谱法分析水基胶中羰基化合物

建立了直接衍生/高效液相色谱分析水基胶中8种痕量羰基化合物(甲醛、乙醛、丙酮、丙烯醛、丙醛、丁烯醛、2-丁酮和丁醛)的方法.对影响分析效率的因素进行了考察,确定最佳衍生条件为:水基胶样品与2,4-二硝基苯肼衍生剂在40℃下反应20 min;最佳色谱分析条件为:采用DIONEX Acclaim Explosives E2...