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.     

High Performance Liquid Chromatographic Assay of phenylbutazone in Pharmaceutical Dosage Forms

Abstract

A simple, rapid and reliable high performance liquid chromatographic procedure for the quantitation of phenylbutazone in pharmaceutical dosage forms was developed, and compared with the U. S. P. XXI method and a spectrophotometric assay developed in this laboratory. A comparison of the three methods indicated that the HPLC method is the most rapid, simple and reproducible. The recoveries based on six placebo samples were 100.2, 99.2, and 99.4% by HPLC, UV and the U. S. P. method, respectively, and their respective CVs were 0.39, 0.73, and 1.5%. Replicate regression analyses of three standard plots in the concentration range of 0.02-0.12 mg/ml obtained using the HPLC assay on three different days yielded a correlation coefficient <0.999 and the coefficient of variation for the three slopes was 1.05%. It is suggested that the proposed HPLC method should be used for routine quality control and dosage form assay of phenylbutazone.     

A New High Performance Liquid Chromatographic Assay for Fluspirilene in Dosage Forms

Abstract

A new method for the assay of fluspirilene (R 6218) in dosage forms using HPLC has been developed. The instrument used had a low volume positive displacement pump, a universal injector, a single wavelength (254 nm) detector, and a data module. The column was stainless steel 30 cm × 4 mm i.d. packed with microparticulate silica. The mobile phase consisted of equal volumes of chloroform and methanol at a flow rate of 1 ml per min. A linear relationship (r = 0.999) was obtained between peak area and concentration of fluspirilene in the range 10–200 μg per ml; no internal standard was used. Fluspirilene was extracted from injectable aqueous suspensions by membrane filtration, drying and dissolution in chloroform-methanol (1:1). Results of assaying fluspirilene in two commercial injectable suspensions by this method were 99.73 and 99.78% of labelled amount.     

High Pressure Liquid Chromatographic Analysis of Orphenadrine Citrate and Acetaminophen in Pharmaceutical Dosage Forms

Abstract

An ion pair reversed phase high pressure liquid chromatographic method for the analysis of orphenadrine citrate (I) and acetaminophen (II) was developed. The mobile phase consisted of 20mM sodium-1-octane sulfonate in 50mM phosphate buffer (pH=3.0), mixed with 22.5% organic solvents (50:50, acetonitrile: methanol). The method is simple, reliable and could be adapted for quality control purposes.     

High Performance Liquid Chromatographic Assay of Verapamil Hydrochloride in Dosage Formsk

Abstract

A stability indicating high-performance liquid chromatographic (HPLC) method for determining verapamil hydrochloride in dosage forms is described. The assay affords baseline separation of the drug from its synthesis impurities and from photolytic degradation products, as well as from formulation excipients. The drug was extracted in 0.05 N hydrochloric acid, chromatographed on a C₁₈ reverse-phase column, eluted with methanol-water-acetic acid-triethylamine (55:44:1:0.1) and the effluent was detected at 280 nm. Linearity studies were carried out using peak height or peak area measurements and the detector response to the concentration of verapamil hydrochloride was confirmed. Excellent interlaboratory precision and recovery data were obtained by the spiked placebo method. This procedure was rapid and selective for the assay of the cardiotonic drug. Application of the method for the assay of verapamil hydrochloride in representative dosage forms is described.     

Simultaneous High Performance Liquid Chromatographic Determination of Theophylline and Ethylenediamine in Aminophylline Dosage Forms as Their Dansyl Derivatives

Abstract

A simple HPLC method has been developed for the assay of the components of aminophylline (theophylline: ethylenediamine 2:1) in solid and liquid dosage forms. Following the extraction of tablets into or the dilution of a liquid dosage form with water, the aqueous extract was reacted with dansyl chloride in an alkaline medium. The mixture of the dansyl derivatives of theophylline and ethylediamine was analyzed on an reversed phase μBondapak Cia column, using a methanol-water-acetic acid-triethylamine (60–65: 33–38: 1. 5:0. 5) mobile phase delivered at the rate of 1.5 mL/min, and a detection wavelength of 254 nm. In addition to exhibiting excellent accuracy and precision, the method yielded detector responses that were linearly related to concentrations of theophylline and ethylenediamine in aminophylline of up to 7 mg of theophylline, and of up to 10 mg     

高效液相色谱分析法测定色氨酸对映体

采用高效液相色谱法,以手性冠醚Crownpak CR( )为固定相、高氯酸溶液/甲醇混合溶液为流动相,成功地实现了色氨酸(Trp)对映体的色谱分离.考察了流动相中甲醇含量、流量和柱温等因素对分离效果的影响.研究表明,适当提高流动相中的甲醇含量、降低流动相流量、降低柱温可以有效地提高分离度.另一方面,提高流动相中的甲醇含量、提高流动相流量、升高柱温可以显著地缩短样品的保留时间.确定了一种最佳分析分离条件,即流动相为甲醇∶高氯酸溶液=15∶85(V/V),流动相流量0.8 mL/min,柱温20℃,波长220 nm,在此条件下进行色谱分离,样品的保留时间小于12 min,分离度达到2.06.该方法具有快速、高效、准确和精密度高等优点.     

高效液相色谱法测定柴油族组成

在银型磺酸键合硅胶柱上以含苯或环己烯的正己烷为流动相,实现了饱和烃、烯烃的基线分离,以改进的迁移丝式氢火焰离子化检测器（ＭＷ－ＦＩＤ）进行定量检测,同时考察了Ａｇ－ＳＣＸ柱的使用性能及改进的ＭＷ－ＦＩＤ的定量准确性。在此基础上建立了高效液相色谱体系分离柴油族组成（饱和烃、烯烃、芳烃及胶质）。     

1-硝基蒽醌的高效液相色谱分析

用Ｖ（Ｎ,Ｎ－二甲基酰胺）：Ｖ（１,４－二氧六环）：Ｖ（二甲基亚砜）＝５：２：１混合溶剂溶解试样,利用Ｗａｔｅｒｓ Ｎｏｖａ－ｐａｋ Ｃ１８色谱柱,以１,４－二氧六环／甲醇／水＝１５／４５／４０（体积比）混合溶液为流动相,对１－硝基蒽醌样品进行了高效液相色谱法分离与分析研究。在所确定的色谱分离体系中,样品中各组分全部出峰且基本上达到基线分离,对定量方法进行了讨论,加标回收率除１,７－二硝基蒽醌外其     

Quantitation of Terbutaline Sulfate in Pharmaceutical Dosage Forms Using High Performance Liquid Chromatography

Abstract

A stability-indicating reverse phase high-performance liquid chromatography method has been developed to quantify terbutaline sulfate in pharmaceutical dosage forms. The method is accurate and precise with percent relative standard deviations based on 6 readings of 0.6 with an internal standard (salicylic acid) and 0.8 without an internal standard. The results are in excellent agreement with the USP-NF method. A decomposed sample gave 49.4% results with the developed method versus 71.3% with the USP-NF method.     

Ion-Pairing High-Performance Liquid Chromatographic Determintation of Pyridoxine and Pyrithioxine in Dosage Forms

Abstract

An ion-pairing High-performance liquid chromatographic method is described for the simultaneous determination of pyridoxine HCI and pyrithioxine 2HCI in dosage forms. A reversed-phase chromatography using tetrabutylammonium hydroxide as the counter-ion was employed. the analysis was carried out utilizing an Aminopropylsilicon-(APS-Hypersil) 5 μm column. Calibration curves were rectilinear over the concentration range 5–40 μg/ml for pyridoxine HCI and 10–100 μg/ml for pyrithioxine 2HCi with minimum detectability (S/N=2) of 0.02 and 0.08 μg/ml respectively. the proposed method was applied to tablets containing the two species, and the results obtained were accurate and precise.     

Oil-in-Water Microemulsion High Performance Liquid Chromatographic Analysis of Pharmaceuticals

Efficient and novel oil-in-water microemulsion HPLC separations of a range of solutes have been achieved using isocratic elution and a conventional reversed-phase HPLC column. A single set of isocratic oil-in-water microemulsion HPLC conditions are shown to be successful for the resolution of a wide range of basic, neutral and acidic drugs and excipients. A robust separation method was developed for the quantitative analysis of Naproxen in a tablet formulation. The method offered a similar run time and improved chromatography when compared to conventional HPLC modes, demonstrating its potential for routine use. In developing the separations the effect on the chromatography of varying the operating parameters was studied. While generally the method was robust to changes in some variables, others markedly changed the separation selectivity, solute retention, peak-peak resolution or resulted in poor chromatographic performance. The method was found to be compatible with very low UV working detection wavelengths. As a final stage to the experimental programme, a microemulsion method was developed with the capability of analysing a range of water-insoluble drugs.     

高效液相色谱法分析蜂蜜中的糖

本文研究了用四乙撑五胺（简称ＴＥＰＡ）作为胺基改善剂，在硅胶柱上定量分析蜂蜜含糖量的方法，并成功地分离了木糖、果糖、葡萄糖、蔗糖、麦芽糖和乳糖。对操作条件进行了探讨。采用示差折光检测器检测，含０．０１％ＴＥＰＡ的乙腈－水（７７＋２３）作流动相。六种糖的相对标准偏差均小于３．５％。     

Determination of Plasticizers Commonly Used In Pharmaceutical Dosage Forms by High Performance Liquid Chromatography

Abstract

A simple reversed-phase HPLC method was developed to identify and quantify plasticizers commonly used with polymers present in sustained or controlled release dosage forms. the plasticizers investigated included triethyl citrate, tributyl citrate, acetyl triethyl citrate, dibutyl sebacate, diethyl phthalate, dibutyl phthalate, and triacetin. the plasticizers were detected at 220 nm, the mobile phase being methanol:water (70:30 v/v%). the peak area response was linear over the studied concentration range of 0.5–5.0 mM/L for triethyl citrate, acetyl triethyl citrate, dibutyl sebacate, and triacetin, and 0.005 ? 0.05 mM/L for diethyl phthalate. the recovery from solvent-cast ethyl cellulose and Eudragit RS 100 films was complete. Two pharmaceutical applications of this assay included the quantitation of plasticizers in polymer-coated sugar beads and a leaching study of a water-soluble plasticizer, triethyl citrate, from polymeric films into simulated intestinal fluids.     

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.     

食品中有机酸的高效液相色谱分析法

对离子交换色谱法、离子排斥色谱法和反相高效液相色谱法分析食品中有机酸的特色和近几年的研究与应用状况作一综述。     

High Performance Liquid Chromatographic Analysis for Free Valine in Plasma

Abstract

A precolumn derivatization method is presented with the use of a fluorescent derivative, 1-dimethylaminonaphhalene-5-sulfonyl-chloride, dansyl chloride, for the detection of free valine in plasma. Dansylated amino acids were determined in deproteinized samples by reverse-phase liquid chromatography. The level of detection is 100 femtoraoles (10^?15). Sample preparation required precipitation of proteins with trichoroacetic acid and removing the excess acid with water saturated ether. The deproteinized sample was adjusted to pH 9.0 and reacted with dansyl chloride. The dansylated products were detected by ultraviolet and fluorescence spectrometry. Elution time for valine subsequent to injection is 25 minutes, while the total assay requires less than 50 minutes.     

聚硅氧烷涂敷的反相高效液相色谱固定相

用甲基乙烯基聚硅氧烷涂敷于硅烷化的微粒硅胶上，制备出一种新型的涂敷型反相高效液相色谱固定相。该固定相对极性、非极性和碱性化合物均有良好的分离能力，峰对称性好。对其恶性循环 了考察，连续使用三个月后，固定相的碳量和色谱性能仍保持不变。     

High Performance Liquid Chromatographic Analysis of Cepoperazone in Serum and Urine

Abstract

A high performance liquid chromatographic method was developed for the quantitative analysis of cefoperazone in serum and urine. Standard curves were linear over the range of concentrations 2–30 μg/ml and a good correlation was established between the amount of cefoperazone injected and peak height. The mean percentage analytical recovery of cefoperazone was 96.3% and the mean within day coefficient of variation in serum was 2.8%. Serum and urine components, as well as several beta-lactam antibiotics, did not interfere with the measurement of cefoperazone. This is a rapid, reproducible, and sensitive assay suitable for use in pharmacokinetic studies.     

High Performance Liquid Chromatographic Analysis of Polymerization Inhibitors in Acrylic Monomers

Abstract

High performance liquid chromatographic methods are described which provide for the quantitative determination of p-hydroquinone in acrolein and p-monomethyl ether of hydroquinone in the ethyl, n-butyl, iso-butyl, and 2-ethylhexyl esters of acrylic acid. The procedures are fast, precise, and applicable to industrial process analyses.