Determination of Steroids in Human Urine by Micellar Liquid Chromatography

Abstract

A simple and sensitive method for the determination of steroids using micellar liquid chromatography is described. The steroids, including hydroxycorticosterone. corticosterone, northisterone, testosterone, mexdroprogesterone acetate and progesterone, were separated by reversed-phase using a micelles mobile phase following UV detection at 245 nm. The parameters affecting retention of the test solutes such as the concentration of sodium dodecyl sulfate (SDS) and n-butanol-1 in the mobile phase were investigated. It was found that the retention of the solutes was dependent on the composition of mobile phase. The linear calibration plots range from 0.1 to 10 μg ml^?1 in mobile phase containing 5.0 × 10^?2 mol l^?1 SDS/9 % n-butanol-1 at pH 6.0, and the detection limit in order of 0.1 μg ml^?1 was obtained. The proposed method was used for the determination of steroids in urine using direct injection of samples without previous treatment.     

A Simple Liquid Chromatography Method for the Determination of Captopril in Urine

A simple and specific method for the determination of total captopril in human urine was developed. 2-Chloro-1-methylquinolinium tetrafluoroborate was used as a thiol precolumn derivatizing reagent after conversion of a disulfide forms to free captopril with tris(2-carboxyethyl)phosphine hydrochloride. The 2-S-quinolinium derivative of captopril was separated on a Zorbax SB C-18 column using reversed-phase ion-paring chromatography and monitored by spectrophotometric detector at 355 nm. The calibration curve for the derivatized captopril showed linearity in the range 0.1–200 μmol L⁻¹ of urine with a regression coefficient corresponding to 0.9999. The detection and quantitation limits were 0.05 and 0.1 μmol L⁻¹, respectively. The intra-day imprecision was from 0.01 to 10.58%. This method can be used for routine clinical monitoring of the thiol-drug. Omission of the reduction step gives result for concentration of the reduced form of captopril.     

毛细管气相色谱法测定电热蚊香液中的丙炔菊酯

采用HP－1毛细管气相色谱法对电热蚊香液中丙炔菊酯的含量进行了定量分析，其测定结果的相对标准偏差为0．3％，回收率为103．05，具 有操作准确、简便，快速和实用等特点。     

高效液相色谱法测定尿液中的异硫氰酸酯

 省去合成1,3 苯二硫杂环五烯 2 硫酮这一步骤，直接用异硫氰酸丙基酯与1,2 苯二硫酚反应作标准，建立了尿液中异硫氰酸酯的反相高效液相色谱(HPLC)测定方法。异硫氰酸丙基酯的标准曲线回归方程 y =0.418 2x + 2.821 ( r2 = 0.999 3 )与异硫氰酸甲基酯的回归方程 y = 0.412 2x + 2.442 3 ( r 2= 0.996 6 )基本拟合。检出限(以信噪比为2.5计)为0.08 μ mol/L 。日内重现性( n =21)以相对标准偏差(RSD)表     

人尿中异黄酮的高效液相色谱分析

建立了测定人尿中异黄酮组分(大豆苷原、黄豆黄素、雌马酚、染料木黄酮)含量的反相高效液相色谱法。在尿样中加入黄酮作为内标,异黄酮经酶解后在pH=7.0中性条件下用乙酸乙酯(1∶1)提取,然后用0.02%TFA-M eOH-ACN三元梯度洗脱的方法分离异黄酮。在该条件下,大豆苷原、黄豆黄素、雌马酚、染料木黄酮的检出限分别为12.9 nmol/L、13.9 nmol/L、71.6 nmol/L和11.8 nmol/L;回收率均在89%以上。本方法具有测试步骤简单、准确度高、重现性好等优点,适合大批量样品测定。     

反相高效液相色谱法测定尿中对氨基苯酚

In this paper, p-aminophenol in urine was separated from its matrix and determined bv RP-HPLC witha fast column of Spherisorb C(18), 3μm, 50×4.6mm i.d.and mobile ohase of MeOH: H2O: H3PO4(22: 78:0.1, V/V/V). The sample was previously undergone hydrolysis,extraction and filtration through 0. 22μm membrane.     

Determination of 3,4-Methylenedioxymethamphetamine (MDMA) and 3,4-Methylenedioxyamphetamine (MDA) in Urine by High Performance Liquid Chromatography

Abstract

The present study proposes a simple, inexpensive method for the identification and quantification of 3,4-methylenedioxymethamphetamine (MDMA) and its principal metabolite 3,4-methylenedioxyamphetamine (MDA) in samples of human urine utilizing high performance liquid chromatography with a UV detector. The optimized method presented adequate linearity, sensitivity, precision, selectivity, and robustness, thereby demonstrating its feasibility for adoption as a laboratorial option for the confirmation of the presence of the drug in urine samples from users.     

Determination of Chlormezanone in Plasma and Urine by High Performance Liquid Chromatography

Abstract

A reversed-phase high-performance liquid chromatographic (HPLC) method with UV detection was developed for quantifying chlormezanone in plasma and urine. an extraction step was needed to avoid endogenous interferences especially in urines and led to an average recovery of 90%. the sensitivity limit was 20 ng/ml in both plasma and urine. the method was reproducible with intra- and inter-assay coefficients of variations below 5%. This method was applied to the determination of plasma and urine levels during a pharmacokinetic study in the elderly. It was found suitable to follow the concentrations as long as 120 h after a single oral administration of 400 mg chlormezanone.     

Determination of Saccharin in Plasma and Urine by High Performance Liquid Chromatography

Abstract

A sensitive and specific high performance liquid chromatographic (HPLC) assay for the determination of saccharin in plasma and urine was developed. Saccharin is extracted into diethyl ether at acid pH, evaporated, and reconstituted prior to instrumental analysis. Overall recovery of saccharin is 86.9 + 8.6% and the sensitivity limits of detection is 0.15 μg per ml of plasma or urine using a fluorescence detector. The sensitivity limit in plasma can be extended to 20 ng per ml by use of a 2 ml assay volume and detector attenuation. The assay was used for the determination of saccharin in plasma and urine of rats following oral doses of 5 mg/kg.     

高效液相色谱法测定小鼠尿中的盐酸戊乙奎醚S型异构体

建立了测定动物体液中S型盐酸戊乙奎醚异构体的高效液相色谱法,研究了S型异构体在小鼠体内的排泄。以Spherisorb SiO2色谱柱(150 mm×4.6 mm i.d.,5 μm)分离S型异构体,外标法定量。S型盐酸戊乙奎醚异构体的线性范围为0.5-100.0 mg/L, 最低检测质量浓度为0.1 mg/L。肌注给药后不同时间内,S型异构体在小鼠尿中的比值(S-1/S-2)存在显著性差异。48 h内各异构体在尿中的排泄量明显不同,说明S型异构体在小鼠体内可能呈现立体选择性排泄。此法简便、经济,可用于动物     

Determination of Catecholamines by Capillary Electrophoresis and Reversed-Phase High-Performance Liquid Chromatography

A method is proposed for the electrophoretic determination of adrenaline, noradrenaline, and dopamine with mass-spectrometric or UV detection. A procedure is proposed for the sample preparation of biological fluids with the use of solid-phase extraction on alumina. A comparative assessment of the determination of catecholamines by capillary electrophoresis and reversed-phase high-performance liquid chromatography was performed.     

Niacin Determination in Legumes by Capillary Electrophoresis (CE). Comparison with High Performance Liquid Chromatography (HPLC)

Available and total niacin content in lentils and faba beans have been analyzed by capillary electrophoresis (CE), and the results compared with those obtained by high performance liquid chromatography (HPLC). Acidic and enzymatic hydrolysis have been carried out for available niacin determination, and an alkaline extraction performed for total niacin. The extracts were subsequently purified using a strong anion exchanger resin. Precise conditions for purification had to be worked out for each one of the two analytical methods (HPLC and CE). The HPLC analysis for available and total niacin was carried out in an ion-pair reverse phase column with UV detection at 261 nm. For the CE separation, the following conditions were employed: a 20 mM sodium tetraborate; 15 mM sodium dodecyl sulfate and 20% isopropyl alcohol solution as separation buffer; 30 kV and 25 or 30°C. Separation was carried out in a 70 cm effective length × 75 μm i.d. fused-silica capillary using on-column UV detection at 254 nm. The results obtained by CE for lentils and faba beans were similar to those obtained by HPLC.     

糖尿病患者尿液中常见药物含量的高效液相色谱法测定

建立了高效液相色谱/二极管阵列检测法同时测定糖尿病患者尿液中二甲双胍、格列吡嗪和替米沙坦3种常用药物含量的方法.室温条件下以2.5 mmol/L十二烷基硫酸钠-20 mmol/L磷酸二氢钠(pH 4.6)-乙腈为流动相,梯度洗脱,实现了3种药物的有效分离.采用3种不同检测波长,测得二甲双胍、格列吡嗪和替米沙坦的检出限分...     

高效液相色谱法测定猪尿中克伦特罗对映异构体残留量

建立了测定猪尿中克伦特罗对映异构体残留量的高效液相色谱分析方法.在碱化的条件下,用乙酸乙酯提取10 mL猪尿样品,提取液经稀HCl反萃取,萃取液直接过SCX固相萃取小柱,再用5%氨化甲醇洗脱,洗脱液经氮气吹干后用200 μL甲醇定容.采用Astec CHIROBIOTICTM V手性色谱柱,以V(甲醇)∶ V(冰乙酸)∶ V(三乙胺)=99.94∶ 0.02∶ 0.04为流动相进行HPLC分析,检测波长301 nm,外标法定量.克伦特罗单-对映体的峰面积与其浓度在70～5000 μg/L范围内呈良好的线性; 线性相关系数均大于0.9996; 猪尿样品中检出限为0.30 μg/L.猪尿中克伦特罗对映体在1.0～20.0 μg/L范围内的添加回收率为76.3%～91.5%; 相对标准偏差RSD均小于7%(n=5).     

高效液相色谱法测定人尿中神经鞘氨醇和二氢神经鞘氨醇

建立了一种检测人尿中神经鞘氨醇（So）和二氢神经鞘氨醇（Sa）的高效液相色谱方法（HPLC）。离心分离尿样中的片状剥落细胞,裂解后用乙酸乙酯萃取、邻苯二甲醛衍生,在HPLC系统中通过梯度洗脱用Nova-PakC18－RP色谱柱（15cm×3．9mm,4μm）分离、荧光检测器检测。So和Sa的检出限均为0．05ng（女性尿样0,075μg/L、男性尿样0．005μg/L）。分析从我国一个村在采集的40份尿样,女性尿样中So、Sa和Sa／So比值分别为1．29－13．58μg/L、0．25－3．13μg/L和0．15－0．25,男性尿样中分别为0．075~3．07μg/L、0.019－0．50μg/L和0．028～0．26。     

The Rapid Determination of Neopterine in Human Urine by Isocratic High-Performance Liquid Chromatography

Abstract

An isocratic high-performance liquid chromatography method is described for the determination of Neopterine eliminated in human urine, using a μ-Bondapak C₁₈ column (300 × 3.9 mm I.D.) and a strongly polar phosphate buffer (pH 6.2) for elution. This analysis requires only 15 minutes and allows very good reproduc-tibility of retention times. This method is well-suited for automation and routine clinical laboratory in order to quantify human urinary Neopterine in healthy subjects and in subjects with malignant disorders.     

高效液相色谱法同时测定尿中新喋呤和生物喋呤

建立了同时分离检测尿中新喋呤（neopterin,NP）和生物喋呤(biopterin,BP)的高效液相色谱（HPLC）-荧光检测方法。采用Hypersil BDS C18柱、甲醇-水(体积比为10∶90)流动相(流速0.5 mL/min)、激发波长360 nm、发射波长 440 nm、柱温20 ℃的色谱条件,同时分离测定了尿中的NP和BP。尿标本经三氯乙酸处理,在4 ℃下,以12000 r/min的速率离心15 min,上清液用碱中和后,取30　μL直接进样。研究结果表明,NP的线性范围为0.12～10     

反相高效液相色谱法测定人尿中的司帕沙星

1 引 言司帕沙星(5－氨基－1－环丙基－7－(顺－3,5－二甲基－1－哌嗪基)6,8二氟＋1,4－二氢－4－氧代－3－喹啉羧酸,SPFX)只能发射微弱的荧光。因此,研究司帕沙星的荧光增敏在临床和药代动力学方面具有重要意义。有关司帕沙星的分析方法已有较多文献报道,有关荧光检测－高效液相色谱测定司帕沙星的方法至今文献报道很少。作者采用亚硝酸氢溴酸为衍生化试剂。对司帕沙星的衍生化荧光增敏进行了研究,发现在酸性介质中,司帕沙星极易被亚硝酸所氧化,继而在溴化亚铜存在下与氢溴酸反应,生成强的荧光物质。据此建立了荧光检测－高…     

Determination of Suramin in Plasma and Urine by Ion-Paired Reverse-Phase High-Performance Liquid Chromatography

Abstract

A high-pressure liquid chromatographic (HPLC) assay has been developed for the quantification of the anti-viral drug suramin (SUR) in human plasma and urine. This assay is simple and accurate, using an isocratic mobile phase in a reverse-phase ion-pairing mode.

This assay was developed for the determination of high levels of suramin in the urine and plasma of patients being treated for the acquired immunodefficiency Syndrome (AIDS). The limit of detection of this assay was 0.25 μg/mL. Congo red (CR) was used as the internal standard with a retention time of 5.9 min, while suramin had a retention time of 13 min.     

尿中L-精氨酸及其甲基化产物的高效液相色谱法测定

用反相高效液相色谱邻苯二甲醛（OPA）柱前衍生荧光检测，可以直接同时分离和定量尿中的L－精氨酸（L－Arg),N^G,N^G－二甲基精氨酸（ADMA）和N^G,N^G-二甲基精氨酸（SDMA）。方法的平均回收率大于97％；含量的上对标准差低于4．6％；而保留时间的相对标准差低于0．32％；信噪比为3：1时，其检测限为0．3pmol.用该方法测定了正常人和肾肾衰者尿中L－Arg,ADMA和SDMA的含量。