毛细管电泳电化学发光用于丙吡胺及其与血浆蛋白结合率的测定

本实验利用透析袋平衡透析、毛细管电泳Ru(bpy)2+3电化学发光检测技术测定了丙吡胺和人血浆蛋白的结合率.在恒电位1.3 V;进样电压10 kV持续10 s,分离电压15 kV,运行缓冲液30 mmol/L 磷酸盐缓冲液(pH 7.5),检测池中为5 mmol/L Ru(bpy)2+3 稀释于50 mmol/L 磷酸盐缓冲液(pH 7.5)中等最优化的条件下,丙吡胺的检出限为10 μmol/L(S/N=3).对蛋白结合率的测定结果表明,人血浆中的药物浓度为1.6～8.2 mmol/L,丙吡胺与血浆蛋白的结合是呈线性的,其线性回归方程为y=-0.07+0.93x,线性相关系数r为0.9999,丙吡胺与人血浆蛋白的结合率约为90.4%.     

Differential Measurement of Cortisol and Cortisone in Human Saliva by HPLC with Uv Detection

Abstract

Both cortisol and its dehydro metabolite cortisone are present in normal human saliva. A method for differential Measurement of both compounds in 1 ml samples of saliva by HPLC/UV is described. the method uses an extraction column having a cyclodextrin bonded phase to retain the compounds of interest while allowing elution of interfering compounds. A steroid-bearing fraction is eluted from the cyclodextrin column, dried, reconstituted in a weak mobile phase, and injected on a reversed phase HPLC/UV system provided with an injector-mounted reversed phase extraction column. Samples containing corticosteroid concentrations as low as 0.5 ng/ml can be effectively analyzed by this method.     

Quick and Simple Simultaneous Determination for Some Amino Acids by Reversed-Phase HPLC with Uv Detection

Abstract

A simple and rapid high pressure liquid chromatographic method using an ultraviolet detector for simultaneous analysis of histidine, tyrosin and tryptophan, is presented.

Chromatographic separation is achieved on Spherisorb-5 RP-18 5μm reversed phase column and the mobile phase is the isocratic mixture of aceto-nitrile, methanol and water (5:30:65). the eluted amino acids are detected at 220 nm. the retention time is 1.55 min for histidine, 2.21 min for tyrosin and 2.80 min for tryptophan. the correlation of the integrated peak areas with the concentration of amino acids showed a linear relationship between 0.40 to 9.43 ppm for histidine, 0.24 to 22.6 ppm for tyrosin, and 0.20 to 12.8 ppm for tryptophan per 10μl injection.

Simultaneous analysis of histidine, tyrosin and tryptophan gave reproducible results with a mean coefficient of variation 1.93 pc for tryptophan, 2.29 pc for tyrosin and 3.51 pc for histidine and r² = 0.999. the proposed technique was applied to the analysis of these amino acids in urine samples.     

间接光度高效液相色谱法分析无机阴离子的研究

报导了间接光度高效液相色谱法测定了无机阴离子的新方法，在自己研制的硅基键合阴离子交换柱上，用１．０ｍｍｏｌ／Ｌ苯甲酸钠和０．６ｍｍｏｌ／Ｌ柠檬酸钠为洗脱液，可在１５ｍｉｎ内对Ｈ２ＰＯ４、Ｃｌ，ＮＯ２，ＮＯ３，ＳＯ４等六种阴离子得到较好的分离，对Ｃｌ的最小检测限为４．０ｎｇ。     

高效液相色谱荧光检测法测定福建乌龙茶中痕量硒

本文研究了2,3-二氨基萘(DAN)与Se(Ⅳ)反应,生成4.5-苯并苤硒脑(NSD),利用环已烷萃取反应生成的络合物。将有机相注射入填充有μ一Bondapak C_(18)固定相的色谱柱,以环已烷-四氢呋喃(90:10)为流动相,流速为1.0 mL/min,进行HPLC一荧光检测。测定了福建乌龙茶中的微量硒。方法的精密度和回收度均好。检测限达0.12 ng。     

制剂药品中盐酸雷尼替丁含量测定方法的优化

建立高效液相色谱仪测定盐酸雷尼替丁制剂含量的检测方法。采用磷酸盐缓冲液与乙腈等比混合的流动相等度洗脱,于314 nm检测,外标法定量。盐酸雷尼替丁质量浓度在5～500μg/mL范围内与色谱峰面积线性相关,相关系数大于0.999 9。6次测定结果的相对标准偏差为0.85%,加标回收率为(100±2)%。该法操作简便、清洁高效、准确可靠,可用于盐酸雷尼替丁片和胶囊含量的测定。     

十三种利尿剂的高效液相色谱测定方法

对近几年国际奥委会医学委员会公布的禁用表中新增药物及一系列利尿剂的相关化合物进行了研究，比较了不同的提取方法及回收率，研究了几种药物的排泄情况；建立了同时分析13种利尿剂的高效液相色谱测定方法，检出限小于5ng。     

鸡肉中多种磺胺兽药残留量测定的高效液相色谱-电化学检测法

采用液相色谱电化学法测定了鸡肉中磺胺类药物残留量；磺胺用氯仿提取后，取部分提取液用氮气吹干，残渣溶于KH2PO4中，用正己烷脱脂，水相进样，液相色谱分析用C18柱，流动相为甲醇－0．01mol/L KH2PO4(pH6，体积比25：75），检测电位1．0V；与紫外检测器相比，电化学检测器（ECD）有更高的灵敏度和选择性，ECD的检出限为磺胺嘧啶0.02ng，磺胺甲氧哒嗪0．06ng，磺胺甲基异恶唑0.07ng。     

蒸发光散射检测器HPLC法测定大豆低聚糖

蒸发光散射检测器HPLC法测定大豆低聚糖;HPLC;ELS检测器;梯度洗脱;低聚糖;大豆     

葡萄酒中7种酚酸的色谱电化学分析

建立了同时测定葡萄酒中没食子酸、原儿茶酸、丁香酸、p-香豆酸、咖啡酸、绿原酸和阿魏酸等7种生物活性酚酸的反相高效液相色谱电化学分析新方法,并测定了5种国产不同品牌的葡萄酒.采用HypersilODS色谱柱(250mm×4.0mm,5.0μm),流动相为甲醇-4%醋酸,梯度洗脱,流速为0.8mL/min,工作电压为0.7V,柱温为30℃.实验结果表明,电化学法的检出限比紫外法的检出限低4～600倍.     

Analysis of Spectinomycin by HPLC with Evaporative Light-Scattering Detection

A high-performance liquid chromatographic method with evaporative light-scattering detection (ELSD) has been developed for analysis of spectinomycin and related impurities. Separation of spectinomycin from structurally related impurities was achieved on a C₁₈ column. The optimized mobile phase was 25 mmol L⁻¹ ammonium acetate (pH 7.5)-methanol, 90:10 (v/v), at a flow rate of 0.6 mL min⁻¹. The temperature of the drift tube of the ELSD was 95°C and the flow rate of carrier gas was 2.2 L min⁻¹. The accuracy, specificity, precision, linearity, sensitivity, and robustness of the method were validated in accordance with ICH guidelines. In addition to determination of spectinomycin and related impurities, the method is also ideal for determination of the salts spectinomycin hydrochloride and spectinomycin sulfate.     

Chromatographic Fingerprint Analysis of the Flowers of Abelmoschus manihot Using HPLC with Photodiode Array Detection

Abstract

A simple and valid chromatographic fingerprint analysis method was developed using high‐performance liquid chromatography‐photodiode array detection for the quality analysis of the flowers of Abelmoschus manihot. For the first time, the feasibility and advantages of employing chromatographic fingerprint were investigated and demonstrated for the evaluation of the flowers of A. manihot by systematically comparing chromatograms with professional analytical software recommended by State Food and Drug Administration. Our results revealed that the chromatographic fingerprint combining similarity evaluation could be used efficiently for the identification and quality assessment of raw herbs of the flowers of A. manihot from different sources.     

天然产物黄酮类化合物的高效液相色谱分析

引用了自1997年以来的45篇文献,综述了黄酮类化合物的高效液相色谱（HPLC）分析方法,着重介绍了黄酮、黄酮醇和双氢黄酮等的定性和定量分析,同时简要介绍了指纹图谱及药代动力学研究,为黄酮类化合物今后在分离分析,质量控制和药理药效研究等方面的深入研究提供理论依据。     

Analysis of Nereistoxin Using HPLC And Electrochemical Detection

Abstract

Nereistoxin blocks nicotinic cholinergic transmission, but the exact mechanism by which this dithiolane blocks nicotinic acetylcholine receptors is not clear. One possibility is that nereistoxin is reduced in vivo and the resulting product, dihydronereistoxin, reduces a disulfide bond in the region of the receptor where acetylcholine binds. Other possibilities include that nereistoxin oxalate as supplied is not pure and contains dihydronereistoxin, or that nereistoxin acts as a simple competitive antagonist. We report here a method for simultaneous detection of both nereistoxin and dihydronereistoxin using π reversed-phase, ion-pair high-performance liquid chromatography with electrochemical detection. The standard curve for nereistoxin is linear to 400 pmol, and the detection limit is 10 pmol. The working electrode response is stable for up to 60 injections. Reduction of nereistoxin to dihydronereistoxin by NaBH₄ was 92% complete under the conditions reported here, but reoxidation occurs slowly upon standing at room temperature. No dihydronereistoxin was detected in commercial samples of nereistoxin oxalate.     

硅氟唑对映体在直链淀粉手性固定相HPLC上的拆分

硅氟唑;三[(s)-α-甲基苯基氨基甲酸]直链淀粉酯;手性固定相;HPLC;手性拆分     

HPLC Assay for Trimethoprim in Plasma and Urine

Abstract

A sensitive HPLC method for the quantitation of trimethoprim in plasma and urine was developed using fluorescence detection. Plasma (or urine) samples were made basic by the addition of 3.8N sodium hydroxide and extracted with chloroform:2-propanol (95:5). After evaporation of the organic layer, a portion of the residue was analyzed by HPLC with fluorescence detection. The minimum detectable quantity is 0.1 μg/ml for this method. This method has been applied to the analysis of plasma and urine obtained from subjects after a single 160 mg dose of trimethoprim.     

生物样品中神经递质含量的测定

用反相高效液相色谱 -电化学检测法 ,同时测定了小鼠脑组织以及人血清中的 6种神经递质的含量。以柠檬酸钠缓冲溶液和甲醇作流动相 ,优化后得到最佳色谱条件。在 1～ 2 0 0× 1 0 - 3mg/ L范围内 ,浓度与响应的线性关系良好 ,各待测物的检出限可达 0 .4～ 5.0× 1 0 - 3mg/ L。     

Routine drug level measurements by means of a fully mechanized HPLC equipment

Summary Pharmacokinetic studies require a great number of serum drug levels to be determined. It is therefore necessary to rationalize analytical methods. Methods for rational clean-up procedures and the determination by means of mechanized HPLC are shown. The following quality criteria for determination methods are proposed: precision, accuracy, specificity and sensitivity. Quality control in routine analyses is performed by evaluating the criteria of parallel analyses of known admixtures to serum.     

Liquid Chromatography with Fluorescence Detection in the Analysis of Biological Fluids

ABSTRACT

Liquid chromatography with fluorescence detection is well suited to the analysis of biological fluids, as it combines both selectivity and sensitivity. The determinations are not limited to fluorescent compounds, as non-fluorescent substances can be converted to fluorescent derivatives by appropriate reactions. As a consequence of progress in methodology and of the development of new reagents, a great number of biological substances and drugs can now be successfully analyzed by this technique. Reliable automated procedures using pre-column derivatization are available, in particular for the analysis of amino acids and amines. In addition, systems using short columns, reduced particle size of the stationary phase and ultramicro detector cells represent a promising approach to the analysis of very small volumes of sample.