液相色谱法测定血浆中三环类抗忧郁药物

用高效液相色谱法测定了血浆中４种三环类抗忧郁药物：卡马西平、氯氮平、多虑平和阿米替林。方法采用Ｃ_（１８）色谱柱分离,二极管阵列检测器检测,流动相为甲醇：０．５ｍｏｌ／Ｌ三乙胺－０．５ｍｏｌ／Ｌ冰醋酸的水溶液（９０：１０,Ｖ／Ｖ;ｐＨ７．５）。标准曲线的线性范围为０～１０ｍｇ／Ｌ,相关系数在０．９９以上。方法的最小检出浓度为１０～４０μｇ／Ｌ血浆。血中药物经溶剂萃取后,药物的回收率为７３．６７％～９８．２４％,血中杂质不影响药物的检测。方法简便、快速,适用于临床中毒样品的分析。     

Reversed Phase High - Performance Liquid Chromatographic Analysis of Tricyclic Antidepressants in Plasma

Abstract

A reversed phase HPLC procedure is described for measuring the plasma concentration of four commonly used tricyclic anti-depressants (TCA): amitriptyline, desipramine, imipramine and nortriptyline in the range of 25 to 800ng per ml. The procedure involves rapid extraction, and HPLC analysis using a μBondapak C-18 column at 50°C, and a 254nm detector. Coefficients of variation are less than 5% for within run, and 7% for day-to-day experiments. Detection limits are: desipramine -0.5ng, nortriptyline or imipramine -0.6ng, and amitriptyline -0.7ng. Propoxyphene interferes with amitriptyline while chlorpromazine interferes with clomipramine. The procedure is easily adapted for clinical drug monitoring of TCA.     

A Simple Liquid Chromatographic Method for the Simultaneous Determination of Antidepressants in Pharmaceutical Preparations

Fluoxetine (FT), fluvoxamine (FX), sertraline (ST) and trazodone (TD) are new type of antidepressants acting as selective serotonin reuptake inhibitors (SSRIs). In structures, they all have chromophore and can be easily monitored by UV absorption spectrophotometry. A simple isocratic high‐performance liquid chromatographic method with ultraviolet detection (215 nm) was developed for the simultaneous quantification of FT, FX, ST and TD. The determination range of the method is over 10.0–400.0 μM for each drug. The detection limits (S/N = 3, injection 20 μL) are about 0.1 μM for TD, 0.2 μM for FT, FX and ST. The relative standard deviation and relative error of the method for intra‐ and inter‐day analyses of FT, FX, ST and TD were all below 3.7%. Application of the method to the analysis of FT, FX or ST in pharmaceutical product proved feasible. The method could be used for the quality control assay of the analytes in bulk and in formulations.     

Quantitative High Performance Liquid Chromatographic Determination of Bamipine Combined with Tricyclic Antidepressants and/or Antipsychotics in Pharmaceutical Formulations

Abstract

An advanced reserved phase High Performance Liquid Chromatographic (HPLC) method using UV detection, at 251, is presented for the simultaneous determination of bamipine combined with tricyclic antidepressants and/or antipsychotics in various pharmaceutical formulations. Sample analyses were performed on a bonded reserved-phase C-2,5 μm, 250 × 4.6 mm ID (Lichrosorb RP-2)column using aqueous ammonium acetate at constant ionic strength 0.015 M and acetonitrile 35: 65 as eluent, at a flow rate of 0.9 ml/min. The pH was adjusted to 4.7 with acetic acid. The presence of acetate buffer both shortens the elution time and improves the symmetry of the chromatographic peaks. The retention time was for bamipine, prochlorperazine, trifluoperazine, thioridazine, chlorprothixene, haloperidol, clomipramine, trimipramine 8.83, 11.83, 11.50, 11.08, 10.42, 8.05, 10.25, 9.67 min respectively. Linearity and precision data have been assessed. The method also involves an investigation of the dependence of the capacity ratio k′ on the pH and the polarity of the mobile phase.     

高效液相色谱法快速检测猪组织中泰妙菌素残留

应用高效液相色谱法测定猪组织中泰妙菌素残留.试样经磷酸盐缓冲液(pH 8.0)-乙酸乙酯混合提取,离心后加0.1%酒石酸,40 ℃旋转蒸发,除尽有机相,加正已烷除脂,HLB柱净化后,氮气吹干,0.0125%甲酸溶解后HPLC检测.流动相为乙腈-0.0125%甲酸(42∶ 58,V/V).紫外检测波长为210 nm.对猪肉(猪肝)进行15(25)～500 μg/kg的药物添加回收实验,结果表明,泰妙菌素的平均回收率为80.1%～92.7%; 日内相对标准偏差为2.0%～10.2%;日间相对标准偏差为5.9%～13.9%.按信噪比S/N=3计算,猪肉和猪肝中泰妙菌素的检出限(LOD)分别为4.5和7.5 μg/kg.     

A Simultaneous Analysis by High Performance Liquid Chromatography of Bamipine Combined with Tricyclic Antidepressants and/or Antipsychotics in Dosage Forms

Abstract

A reversed phase high-performance liquid chromatographic method is described for the simultaneous determination of antihistamines, tricyclic antidepressants and anti-psychotics in pharmaceutical formulations and in spiked placebos. The separation was performed on an octadecyl-silica column using acetonitrile: tetrahydrofuran: 0.015 M aqueous ammonium acetate (53:42: 5) as mobile phase. The presence of ammonium acetate both shortens the elution time and improves the symmetry of the chromatographic peaks. Measurements were made at 251 nm.     

高效液相色谱法测定阿卡波糖水解产物中的Valienamine含量

1引言Valienam ine((1S,2S,3S,4R)-1-氨基-5-(羟甲基)环己-5-烯-2,3,4-三元醇),分子式C7H13NO4,是一种由假单孢菌降解井冈霉素获得的假氨基糖,可通过阿卡波糖或井冈霉素水解来制备。它不仅能够有效治疗糖尿病及高血糖所导致的肥胖症,而且还能治疗艾滋病等其它疾病,所以对其的研究和开发已引起全世界生物医学领域的广泛关注。Valienam ine的检测方法主要有糖化酶检测法、紫外分光光度法、质谱法和薄层扫描法等,这些方法都存在难于定量或定量不准确、检测不方便的缺陷。有人用p-硝基氟苯与Valienam ine反应衍生生成N-p-硝基苯-Valienam …     

高效液相色谱－电化学检测法同时测定血浆中5－羟色胺和5－羟吲哚乙酸

A simple and Sensitive method for the simultaneous measurement of serotonin(5-HT)and 5-hydroxyin-doleacetic acid(5-HIAA)in plasma is described.Plasma samples,only deproteinated,without further extraction,were directly injected into and high performance liquid chromatographic column and detected electrochemically. Within 18 min,the total separation was achieved.The recovery reached over 90%. The coefficient of variation inretention time was less than 2.5%and in peak area was less than 1.2%.     

整体柱高效液相色谱法测定尿中核苷的方法研究

尿中修饰核苷已被研究用作可能的肿瘤标记物,目前最常用的分析方法为反相高效液相色谱法,其不足之处是分析周期太长。为此,建立了应用整体柱的高效液相色谱方法对尿中修饰核苷进行分析,所用缓冲液为25 mmol/L磷酸二氢钾溶液(pH 4.55)和60%(体积分数）的甲醇水溶液,线性梯度洗脱,检测波长为260 nm。12种目标核苷可被完全分离。所建立的方法在分离度、线性、重现性、灵敏度及回收率等指标上与普通反相液相色谱法相近,但分析周期大大缩短,仅为23 min,适合于大量临床样品的分析。     

Improved High Performance Liquid Chromatographic Method for the Determination of Some Corticosteroids

Abstract

A simple, selective and accurate high performance liquid chromatographic method for the determination of some pharmaceutically important corticosteroids has been developed. the suggested method uses a ultrasphere ODS column with acetonitrile-phosphate buffer (pH 8) as a mobile phase.

The mean percentage recovery ranged from 97.9 to 99.7, the proposed method was applied to the determination of the studied corticosteroids pro in some dosage forms. the statistical analysis of the results obtained were compared favourably with those given with the official method.     

高效液相色谱/荧光检测法同时测定高分子材料中6种异氰酸酯

建立了高分子材料中6种异氰酸酯含量的高效液相色谱/荧光检测法。样品中的异氰酸酯经萃取衍生,C18色谱柱梯度洗脱分离后,以荧光检测器检测,外标法定量。考察了萃取剂、萃取方式、衍生化时间及流动相组成对异氰酸酯萃取量、衍生化效果及分离效果的影响。结果表明,选用极性萃取剂二氯甲烷超声萃取的回收率高于非极性萃取剂环己烷振荡萃取的回收率,最佳衍生化时间为30 min。流动相采用乙腈-三乙胺缓冲液梯度洗脱时,目标组分的分离度高于1.5,在10~100 μg/L范围内异氰酸酯衍生物的线性相关系数不低于0.999 1。高分子样品中异氰酸酯的加标量在0.1~1.0 mg/kg范围内,平均回收率为90%~95%,相对标准偏差(RSD,n=5)为2.2%~4.2%。检出限(信噪比为3)为30.3 ~42.3 μg/kg。实际样品检测结果表明,除苯基异氰酸酯(PI)外的5种异氰酸酯在样品中均有不同程度检出,总含量为79.7~326.3 μg/kg。该方法准确、灵敏、重现性好,适用于高分子材料中异氰酸酯残留量的检测。     

A New Bonded-Phase for High Performance Liquid Chromatographic Analysis

Abstract

A silica bonded-phase with carboxylic acid functionality and a side chain of three carbon atoms has been synthesized for HPLC analysis. Mixtures of nucleic acid bases, PTH-amino acids, phospholipids and ethanolic extract of dry ginger powder were analyzed to demonstrate its performance. Nucleic acid bases and PTH-amino acids were separated by cation-exchange mechanism whereas phospholipids experienced combination of cation-exchange and normal-phase resolution. The resolution of gingerols in the dry ginger powder was achieved by reversed-phase mechanism.     

高效液相色谱法测定西红柿中克线磷残留量

高效液相色谱法测定西红柿中克线磷残留量包宏,夏民洲,胡兹苓（南京林业大学南京２１００３７）１前言克线磷（ｆｅｎａｍｉｐｈｏｓ）,商品名Ｎｅｍａｃｕｒ,是防治作物根结、孢囊与自由线虫的杀线虫农药￣［１］。对它的残留分析,有气相色谱法和薄层色谱法等￣［２...     

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.     

高效液相色谱法同时分析低浓度的葡萄糖、乙醇和甘油

 用高效液相色谱法同时分析、示差折光检测器检测酿酒酵母发酵液中的葡萄糖、乙醇及甘油。方法快速、灵敏、操作方便。同时利用高效液相色谱法对酿酒酵母细胞群体发酵初期的代谢行为进行了初步研究。     

高效液相色谱法测定血中苯妥英浓度

A high performance liquid chromatographic method for the quantitative analysis of phenytoin(PHT) inhuman plasma or whole blood is described. After a onestep extraction of PHT and internal standard withethyl acetate from human plasma or whole blood,samples were chromatographed on a Spherisorb-C(18) columnwith a mobile phase of methanol-water-tetrahydrofuran(45/55/5,V/V/V)at a flow rate of 0. 3mL/min. Theeluant was monitored at 210nm.     

高效液相色谱-荧光检测法同时测定蔬菜中3种磺胺类药物残留

建立了蔬菜中3种磺胺类药物(SAs)的高效液相色谱-荧光检测法。蔬菜样品用甲醇提取3次,将提取液浓缩干,用0.1mol/LHCl溶解残渣,经荧光胺衍生化后,用反相柱(ODS)分离,以乙腈和0.5%醋酸为流动相进行梯度洗脱,用荧光检测器检测。3种SAs的检出限(LOD)为1.02～1.29μg/g,方法的定量限(LOQ)为3.4～4.3ng/g(鲜重)。蔬菜样品中SAs的添加浓度在0.2～1.0ng/g范围内,3种SAs的平均回收率均大于87%,日内与日间RSD均小于10%。实际蔬菜样品测定结果表明,3种SAs在不同蔬菜中均有不同程度检出,总含量为0.0726～0.3709μg/g(鲜重)。     

Simultaneous Determination of Six Anticonvulsants in Serum by High Performance Liquid Chromatography

Abstract

The authors describe a simultaneous determination method of six anticonvulsants (ethosuximide, primidone, phenobarbital, phenytoin, carbamazepine, valproic acid) using 500 μl of serum.

After the addition of the internal standard (5-(p-methylphenyl)-5 phenylhydantoin), the anticonvulsants are extracted in an acid medium with ethyl acetate. They are separated by reverse phase chromatography on a μ Bondapack C18 column, eluted with a water/methanol mixture (36/64 V/V) at a flow rate of 0.7 ml/min.

The column effluent is first analyzed by monitoring the ultraviolet absorption at 197 nm and then at 425 nm after the addition of a color indicator: bromocresol purple. The analysis lasts 12 minutes at ambient temperature. The sensitivity obtained with the serum for the range of products investigated is of the order of 0.5 to 2 mg/l, the extraction recoveries varying from 75 to 100% depending on the drug. Reproducibility is good (cv ≤ 9%).     

植物中鱼藤酮类化合物高效液相色谱检测方法的改进

1　引　　言由于生产上对高效、低毒、低抗性的植物源杀虫剂的需要 ,以及近年发现其有抗癌活性 ,鱼藤酮类 (ｒｏｔｅｎｏｉｄｓ)化合物的研究再次受到国内外重视。该类化合物主要来源于豆科的鱼藤属、灰毛豆属、合生果属、鸡血藤属、紫穗槐属、黄檀属、毒鱼豆属和蝶豆属等植物 ,迄今已发现的鱼藤酮类化合物在 74种以上。现有的ＨＰＬＣ分析方法均是针对鱼藤酮而设计的 ,对其它类似化合物的分析存在一定局限性。建立适合植物中鱼藤酮类化合物的ＨＰＬＣ分析方法对植物或提取物中各组分的分离分析和含量测定有重要意义 ,是获得评价其质量、加…     

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。