高效液相色谱-化学发光方法同时测定血清中的肾上腺素、去甲肾上腺素和多巴胺

本文基于肾上腺素、去甲肾上腺素和多巴胺对鲁米诺-铁氰化钾化学发光体系的增敏作用，建立了一种高效液相色谱分离-化学发光检测体系同时检测三种物质；研究了试剂浓度、酸碱条件、流动相成分等参数对分析结果的影响。在优化发光条件下，以邻苯二甲酸氢钾-甲醇溶液（92：8）为色谱流动相，用C₁₈柱分离检测肾上腺素、去甲肾上腺素和多巴胺样品，肾上腺素线性范围为1×10^-8~5×10^-6g/mL，检测限4.0×10^-9g/mL；去甲肾上腺素线性范围是 5.0×10^-9~1.0×10^-6g/mL，检测限1.0×10^-9g/mL；多巴胺线性范围为5.0×10^-9~1.0×10^-6g/mL，检测限8.0×10^-10g/mL。本方法快速、简便而准确，且已成功用于血清中三种物质的分析。     

反相高效液相色谱法测定绿麦隆

反相高效液相色谱法测定绿麦隆王以燕,孙绮丽,张百臻（农业部农药检定所,国家农药质量监督检测中心北京１０００２６）１前言绿麦隆（ｃｈｌｏｒｏｔｏｌｕｒｏｎ）是一取代脲类麦田除草剂,它具有选择性内吸传导作用,目前是我国广泛使用的除草剂之一。绿麦隆分析方法...     

高效液相色谱-电化学检测法同时测定人血浆中的组织胺和去甲肾上腺素

报道了用高效液相色谱配合电化学检测器同时分析组织胺（Ｈｉｓｔ）和去甲肾上腺素（ＮＡ）的方法。用邻苯二甲醛（ＯＰＡ）进行柱前衍生,流动相为Ｖ（乙酸钠缓冲溶液）Ｖ（乙腈）＝７３,检测器电位＋０．７Ｖ,线性范围为０．０１５～５μｇ／Ｌ（ｒ＝０．９９８）,平均回收率为９５％。方法灵敏、准确,重复性好,分析速度快,可用于临床检测。     

痕量硝基酚的反相高效液相色谱电化学检测

本文以甲醇与０．０３ｍｏｌ／Ｌ邻苯二甲酸氢钾缓冲液为淋洗液，采用安培型电化学检测，实现了２－硝基苯酚，３－硝基苯酚，４－硝基苯酚及２，４－二硝基苯酚和２，６－０二硝基苯酚等五种酚类化合物于Ｐｅｒｋｉｎ－Ｅｌｍｅｒ Ｎｕｃｌｅｏｓｉｌ Ｃ８柱上反相高效液相色谱的分离及在Ｅ＝＋１．２Ｖ时于玻碳电极上的同时检测。     

毛细管电泳法同时测定血清中的左旋多巴和甲基多巴

建立了毛细管电泳-紫外检测同时测定血清中左旋多巴和甲基多巴的方法。以40 mmol/L硼砂（pH 9.5）为分离缓 冲溶液,在3.45 kPa（0.5 psi）压力下进样7 s、分离电压22 kV、检测波长200 nm、温度25 ℃的条件下进行测定,两 种物质获得了较好的分离。甲基多巴和左旋多巴分别为1.0~64.0 mg/L和1.0~71.0 mg/L时与峰面积呈良好的线性关系, 线性相关系数分别为0.9998和0.9994,检出限分别为0.6和0.8 mg/L(以信噪比为3计)。将该法用于血清中甲基多巴和左 旋多巴的测定,回收率为82.8%~88.8%,相对标准偏差为2.10%~2.63%。     

反相高效液相色谱法测定碘

建立了碘的反相高效液相色谱测定方法。色谱条件为：Ｓｈｉｍ－ｐａｃｋ ＣＬＣ－ＯＤＳ柱；流动相为甲醇－水（２０：８０）；流速为１ｍＬ／ｍｉｎ；检测波长为２９０ｎｍ。本方法的线性范围为０．１０￣１０ｍｇ／Ｌ；相对标准偏差为１．１％￣１．４％；加标回收率为９７％￣１０１％。所建立的方法已用于医用碘酒的测定。     

反相高效液相色谱法分析巴咯地尔原料药及其制剂

Buflomedil is a new drug used for the treatment of cerebral vascular disease。The determination methodhas not been found in any pharmacopeia,This paper provides a convenient method by using reversed-phaseion-pair chromatography.The column is Hi-pore Rp- 318.The mobile phase is 0.005mol/L sodium laurylsulphate in methanol-water-glacial acetic acid(70:30:0.1).The internal standand is 1,3,5- trimethoxy- benzene。The detection limit is 0. 1 μg/mL and the linear range is 0.05～0. 30 mg/mL。     

蘑菇组织催化氧化-流动注射荧光法测定去甲肾上腺素和左旋多巴

研究发现富含多酚氧化酶的蘑菇组织可催化溶解氧氧化去甲肾上腺素和左旋多巴在碱性条件下生成具有强荧光的三羟基和二羟基吲哚类物质 ,建立了以蘑菇组织柱为酶反应器的去甲肾上腺素和左旋多巴的流通式荧光分析法 .该法对去甲肾上腺素和左旋多巴响应的线性范围分别为 6× 10 -8～ 1× 10 -5g·mL-1和 3× 10 -8～ 1× 10 -5g·mL-1,检测限分别为 2×10 -8g·mL-1和 1× 10 -8g·mL-1( 3S/k) .该组织反应器可连续使用 14d ,对 1× 10 -7g·mL-1去甲肾上腺素和 1× 10 -7g·mL-1左旋多巴测定的相对标准偏差 (R .S .D .)均小于 3 % (n =11) .详细研究了常见离子和抗氧化剂对本体系的干扰情况 .将该体系用于药物制剂中去甲肾上腺素和左旋多巴含量的测定 ,结果与药典标准方法测得值一致 .实验结果证明了方法的可行性和可靠性     

胶束电动毛细管色谱安培检测中药马齿苋中多巴胺和去甲肾上腺素

建立了胶束电动毛细管色谱结合电化学安培检测同时分析中药马齿苋中多巴胺和去甲肾上腺素的方法。考察了缓冲液的浓度、pH值、十二烷基硫酸钠(SDS)浓度以及工作电极电势对分离检测的影响。在优化的条件下,多巴胺和去甲肾上腺素在1.0×10-6～5 0×10-4mol/L范围内有良好线性,浓度检测限(S/N=3)分别为8 7×10-7mol/L和4 2×10-7mol/L,质量检测限分别为1 45fmol和0 41fmol。该方法组分定性可靠,不需要衍生处理,选择性好。将该法应用于中药马齿苋样品的分析,获得了较好的结果。     

High Performance Liquid Chromatographic Determination of Nordihydroguaiaretic Acid

Abstract

A high performance liquid chromatography (HPLC) method was developed for the detection and quantitation of nordihydroguaiaretic acid (NDGA). Very low concentrations of NDGA in various extracts are detectable, thus making the method more sensitive than other previously reported analytical techniques. NDGA was extracted from leaves of Larrea divaricata as well as from rodent food containing NDGA. Since rats are fed NDGA in studies that examine the development of renal cystic disease, we modified extraction procedures to permit isolation of NDGA from tissue and serum samples.     

Rapid High Performance Liquid Chromatographic Determination of Ampicillin in Human Urine

Abstract

A rapid, sensitive and specific HPLC assay for the determination of ampicillin in human urine is developed.

Ampicillin was directly measured in human urine at 225 nm using a reversed phase column (Synchropack RP-P) and a mobile phase composed of (1:9 methanol-sodium acetate solution, 0.01 M, pH 4). The analysis required no longer than 10 min. Linear correlation between the peak height ratio of ampicillin to cefoxitin sodium (internal standard) and ampicillin concentration in urine over the range 10–100 μg ml^?1 was obtained. The developed method proved to be advantageous as it monitors ampicillin level in urine. Moreover, the urinary excretion of ampicillin in human subjects after an oral administration of 500 mg ampicillin capsules was established using the proposed method.     

LC–ESI/MS Analysis of Levodopa and Methyldopa (IS) in Beagle Dog Pharmacokinetic Study after Oral Administration and Domperidone Given in Advance

A simple, sensitive and accurate method was developed for the quantification of levodopa and methyldopa (IS) in beagle dog plasma by LC–ESI/MS, chromatographic separation was carried out by a Diamonsil C18 column (150 mm × 4.6 mm i.d., 5 mm) with an ODS guard column maintained at 30 °C. The mobile phase was methanol (A) and 0.5% formic acid aqueous solution (B) system in the gradient elution profile, the retention time of levodopa and IS were 4.8 and 6.1 min, respectively, linear range for levodopa concentration was 0.08‐20.0 μg/mL in plasma samples with a correlation coefficient(r) of 0.9978, the limit of detection was 32 ng/mL. CV of intra‐day and inter‐day assays were all less than 15%, mean recoveries of levodopa were all more than 90% in 0.32, 1.6 and 16.0 μg/mL concentrations of levodopa (n = 3). The validated method was successfully applied to the determination of levodopa in plasma samples, pharmacokinetic of levodopa following a single oral dose of compound levodopa tablets and antiemetic drug – domperidone administrated to beagle dogs has been carried out, the main pharmacokinetic parameters of levodopa with domperidone were as follows: T_max (0.50 ± 0.18) h, C_max (39.72 ± 7.91) μg/mL, t_l/2 (0.65 ± 0.07) h, AUC_o‐t (49.01 ± 12.13) μg·h/mL , AUC_o‐∞ (49.10 ± 12.16) μg·h/mL, we also evaluated the effect of domperidone on pharmacokinetics of levodopa in beagle dog. We thought non‐oral sustained‐release formulations should be a very good choice instead of this common oral dosage forms on the market, the test results can provide a reference for clinical trials on drug therapy of Parkinson‘s disease.     

High Performance Liquid Chromatographic Determination of Amiodarone in Plasma and Tissues

Abstract

A simple and rapid high-performance liquid chromatographic (HPLC) method for the determination of amiodarone (AD) in plasma and tissues was developed. The method involved deproteinization of plasma or homogenized tissue with acetonitrile containing an internal standard (N-Cetylpyridinium chloride) followed by reversed phase chromatography using μ bondapack C₁₈ column (10μm) with a mobile phase consisting of acetonitrile - methanol - sodium dihydrogen phosphate buffer (70:10:20%, v/v), the pH adjusted to 4.0 and pumped at flow rate of 1.0 ml/min. The column effluent was monitored at 242 nm. A linear relationship was obtained between peak height ratios (drug to internal standard) versus drug levels over the concentration range of 50–750 ng/ml. The detection limit of AD in plasma and tissues by this method was 20 ng/ml.     

基质固相分散－高效液相色谱法测定玉米中痕量呋喃丹

本文研究了应用基质固相分散（ＭＳＰＤ）－高效液相色谱法测定玉米中痕量呋喃丹残留物的新方法，并讨论了应用ＭＳＰＤ技术进行前处理与传统残留分析的区别。本实验首次将ＭＳＰＤ技术用于玉米中呋喃丹残留物的高效液相色谱分析，并对定量检测条件作了详细的研究。     

High Performance Liquid Chromatographic Determination of Triazolam in Human Serum

Abstract

A high performance liquid chromatographic method which utilizes UV-detection has been developed for the sensitive and specific determination of triazolam in human serum. Using 8-chloro-6-phenyl-l-ethoxymethyl-4H-s-triazolo[4, 3-a][1, 4]benzodiazepine as an internal standard, serum samples were buffered with 2 ml of 4M NaOH and extracted twice with 5 ml aliquots of toluene. The combined toluene extracts were evaporated to dryness and the residue dissolved in the chromatographic mobile phase. The samples were chromatography on a microparticulate reverse-phase column using a 0.06M acetic acid:acetonitrile (61:39) mobile phase. Known metabolites of triazolam did not interfere in the analysis. A linear relationship between peak height ratios and concentrations was observed, with the lower limit of detection being approximately 1 ng of triazolam. The utility of the method was demonstrated by administering therapeutic doses of the drug to human volunteers and monitoring serum triazolam concentrations as a function of time.     

芝麻中芝麻素含量的高效液相色谱法测定

建立了一种快速、简便测定芝麻中芝麻素含量的方法。将芝麻粉碎后用甲醇超声提取,优化了粉碎粒径、超声料液比和提取时间。结果表明,芝麻样品经粉碎及超声萃取后,采用高效液相色谱法(HPLC)测定,色谱柱为C18(4.6 mm×250 mm,5μm),流动相为甲醇-水(75∶25),流速1.0 mL/min,柱温30℃,检测波长286 nm。芝麻素在0.043 84~0.569 9μg范围内线性关系良好,回归方程为A=1 346 015m+2 136,r2=0.999 9;芝麻素的加标回收率为100%,RSD为1.1%,不同产地芝麻中的芝麻素含量测定结果为0.260%~0.502%。该方法具有操作简便、稳定、专属、可重复的特点,可用于芝麻的质量控制。     

High Performance Liquid Chromatographic Determination of Flurbiprofen in Pharmaceutical Dosage Forms

Abstract

A rapid, specific and reliable high performance liquid chromatographic assay of flurbiprofen in dosage forms has been developed. Reversed-phase chromatography was conducted using a mobile phase of 0.05 M ammonium acetate and acetonitrile, (40% v/v) PH 5.2 and detection at λ 247 nm. The recovery and coefficient of variation from six placebo tablets spiked with 100 mg of flurbiprofen were 100.1% and 0.4% respectively. Replicate regression analyses of three standard plots in the concentration range 0.5 - 9 mcg/ml obtained on three different days gave a correlation coefficient (0.99996) and the coefficient of variation of the slopes 0.159%. The assay was precise within day and between days as indicated by ANOVA test. It is suggested that the proposed HPLC method should be used for routine quality control and dosage form assay of flurbiprofen.     

First Report for Electrochemical Determination of Levodopa and Cabergoline: Application for Determination of Levodopa and Cabergoline in Human Serum,Urine and Pharmaceutical Formulations

The electrochemical oxidation of levodopa on the surface of a carbon paste electrode modified with graphene nanosheets, 1‐(4‐bromobenzyl)‐4‐ferrocenyl‐1H‐[1,2,3]‐triazole (1,4‐BBFT) and hydrophilic ionic liquid (n‐hexyl‐3‐methylimidazolium hexafluoro phosphate) as a binder is studied. It has been found that the oxidation of levodopa at the surface of a modified electrode occurs at a potential of about 210 mV less positive than that of an unmodified carbon paste electrode (CPE). The prepared modified electrode exhibits a very good resolution of the voltammetric peaks of levodopa and cabergoline. The electrode has been applied successfully for the determination of levodopa and cabergoline in some real samples.     

Specific and Sensitive High Performance Liquid Chromatographic Determination of Alprazolam or Triazolam

Abstract

A specific and highly sensitive liquid chromatographic procedure has been developed for the rapid determination of intact alprazolam or triazolam in dog serum, using these structurally similar triazolobenzodiazepines as mutual internal standards. The procedure consists of (1) extracting one ml of alkali buffered serum with toluene, (2) evaporating an aliquot of the toluene to dryness, and (3) quantitating the redissolved residue by HPLC using ultraviolet detection (221 nm). Samples were chromatographed on a microparticulate reverse phase column using a mobile phase composed of acetonitrile: isopropanol: water (94:5:1) and a flow rate of 0.75 ml/min. Metabolites of alprazolam and triazolam did not interfere in the assay. The lower limit of detection was approximately 1 ng/ml of serum extracted. The utility of the analytical methodology for the determination of alprazolam or triazolam in pharmacokinetic studies in the dog was demonstrated.