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 Determination of Phenacemide in Biological Fluids

Abstract

A sensitive and reliable high performance liquid chromatographic procedure has been developed for the quantitation of phenacemide in plasma or urine. After simple extraction of the drug with ethylacetate from alkalinized samples and evaporation to dryness, the reconstituted extract was chromatographed using a C₈ reversed phase analytical column with UV detection at 254 nm. Regression analyses for the calibration plots obtained on 3 different days for the drug concentrations ranging 1–15 mcg/ml indicated excellent linearity (r >0.999) and reproducibility (CV< 4%, p >0.01). The mean recovery of spiked phenacemide in plasma and urine from the lower limit of quantitation (1 mcg/ml) to 15 mcg/ml was 97.9 and 96.3%, respectively and their respective CV was 3.53 and 2.58%. The method was applied to monitor the plasma vs. time profile of the drug following a single bolus IV dose of 12 mg/kg in a dog.     

High Performance Liquid Chromatographic Determination of Oxamniquine in Plasma Samples

Abstract

A sensitive and reliable liquid chromatographic assay procedure for the quantitation of oxamniquine in plasma or urine was developed. Chromatographic separation was achieved on a reversed-phase phenyl colum using U.V. Detection at 254 nm. The eluting solvent was the mixture of 0.05 M acetate buffer pH 5 and acetonitrile (3:7). With this mobile phase the drug and its external standard were well separated from the interference of the blank samples. The average recovery of oxamniquine from 3 or more replicate dog plasma samples of different concentration (0.125 ? 4.00 μg/ml) was 95.5% and its coefficient of variation was 4.17%. The reproducibility of the assay was confirmed by the analysis of variance test for the slopes of the three standard plots obtained from plasma samples at three different occasions (F=4.2, p > 0.01). The detection limit for plasma samples was approximately 20 ng/ml. The method was applied to measure the plasma level vs, time profile of this drug following a single bolus intravenous dose of 16 mg/kg to a dog.     

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 Hydromorphone Hydrochloride Injection

Abstract

A stability indicating high performance liquid chromatographic (HPLC) method for determining hydromorphone hydrochloride in dosage forms is described. The drug was chromatographed on a C₁₈ reverse phase column, using a mobile phase consisting of sodium lauryl sulfate, acetic acid, acetonitrile and water, and detected at 280 nm. Linearity of detector response to the concentration was confirmed. The procedure showed excellent reproducibility and gave quantitative recoveries of the drug from spiked placebos. Photodegraded samples of the dosage form, were assayed by the HPLC procedure and the current USP spectrophotometric procedure. Comparison of the results showed that the USP procedure is only partially stability indicating.     

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.     

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.     

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 Performance Liquid Chromatographic Assay for Adinazolam Mesylate in Rodent Feed Mixtures

Abstract

Adinazolam mesylate was recovered from the feed mixtures by repeated extraction with a pH 4 citrate buffer. The pooled extracts were diluted with water when necessary and mixed with an equal volume of an acetonitrile solution of internal standard (naphthalene). After mixing and centrifugation, the clear supernates were separated for chromatography. The chromatography was carried out on a reverse phase column using a mixture of phosphate buffer, acetonitrile and methanol in the volume ratios of 85:40:20 as mobile phase. Adinazolam and the internal standard were eluted from the columns at about 11.7–12 and 15.50–17.5 minutes, respectively.

The peak height ratios and adinazolam mesylate concentrations showed excellent linearity (r>0.999). Extracts of blank feed samples did not show interference to the assay. Assay results with satisfactory accuracy and precision were obtained. The methodology was applicable for the assay of the drug-feed mixtures containing 0.02 to 10.0 mg of adinazolam mesylate per gm of feed.     

Liquid Chromatographic Assay for Amodiaquine in Tablets and Biological Fluids

Abstract

A high performance liquid chromatographic assay for quantitating amodiaquine (A) in tablets, urine, plasma, bile and saliva is described. The method involved acid extraction of the drug from tablets and chloroform extraction of its base from the biological fluids after alkalinization with ammonia. Quinidine was used as the internal standard. A μ-Bondapak phenyl column was used for separation together with a mobile phase made of methanol, water and glacial acetic acid (pH 2.3). Good chromatograms with efficient separation of drug and internal standard peaks were observed. Retention times of 5.2 and 7.1 min. were obtained for the drug and the internal standard respectively. Correlation between areas under the curve and drug concentration was high. The mean percentage recovery of A from tablets was 102.03%, while from the biological fluids, it ranged from 85.2 to 104.61%. Urine and saliva obtained from volunteers and bile obtained from animals administering amodiaquine showed chromatograms similar to those obtained for blank samples spiked with A. Interference from table't excipients of biological fluids was undetectable or negligible. The method was found to be precise and simple.     

A Stability Indicating High Performance Liquid Chromatographic Assay of Isradipine in Pharmaceutical Preparations

Abstract

A high performance liquid chromatographic procedure has been developed for the assay of isradipine in bulk form and tablet and capsule pharmaceutical preparations. The separation is achieved within 20 min on an octadecylsilane column at ambient temperature with a mobile phase of 60:40 v/v methanol - water, a flow rate of 1 mL/min, and detection at 325 nm. Degradation studies showed no peak interference between isradipine and degradation products. It was also determined that the excipients in the commercial tablet and capsule preparations did not interfere with the assay. The method was linear in the range 10–60 μg/mL with accuracy and precision in the 0.40 - 1.53% range.     

Improved and Rapid Liquid Chromatographic Determination of Indomethacin in Serum

Abstract

A rapid, specific and sensitive reversed-phase liquid chromatographic (LC) assay for the quantitative determination of indomethacin in serum without extraction was developed. Chromatographic separation using flunixin meglumine as the internal standard was achieved on octadecylsilane-coated particles with a mobile phase of 0.15 M acetate buffer pH 3.0 (50% v/v), acetonitrile (30% v/v) and methanol (20% v/v). The recovery of indomethacin from serum samples in the concentration range of 0.1-25 μg/ml was 95.5 ± 5.8% and as little as 100 ng/ml of indomethacin in serum samples can be quantitated by this procedure. A serum level versus time profile of dog with intravenously administered indomethacin demonstrated the applicability of the assay.     

返魂草的高效液相色谱法指纹图谱研究及成分分析

采用高效液相色谱法,建立了返魂草的指纹图谱,并与相同条件下获得的同属植物千里光图谱进行了比较;通过液相色谱-质谱联用法及与对照品比照研究,对其5种共有成分进行了鉴定;并对以上成分的含量进行同步测定。结果表明,此指纹图谱能够用于区分返魂草及其混淆品千里光;5种成分在各自的浓度范围内线性关系良好(r=0.9995～0.9998),10批样品中原儿茶酸、绿原酸、咖啡酸、金丝桃苷、异槲皮苷含量分别为0.03～0.07 mg/g,0.10～1.04 mg/g,0.01～0.05 mg/g,0.07～0.35 mg/g和0.02～0.74 mg/g。本方法可用于返魂草的鉴别及药材的质量评价。     

Reverse-Phase High Performance Liquid Chromatographic Determination of Clidinium Bromide and Chlordiazepoxide in Tablet Formulations

Abstract

Clidinium bromide is a quaternary ammonium anticholinergic agent with peripheral effects. It is commercially available in combination with chlordiazepoxide. There is no official compendial method available for the analysis of both compounds concurrently. Conventional methods for determining both compounds involve extensive extraction and thus are time-consuming, and lack precision. The analytical scheme described in this paper provides a fast and reliable reverse-phase HPLC for chlordiazepoxide and clidinium bromide in pharmaceutical combinations. The mobile phase was 0.04 M ammonium acetate in 70% acetonitrile solution with 1% dimethylformamide (pH 6). The column was microPak MCH-10 (300.0 mm × 4.0 mm), UV detection at 254 nm and benzophenone was used as internal standard. The method was confirmed for linearity, recovery, specificity, accuracy, and applicability.     

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。     

A Rapid High Pressure Liquid Chromatographic Assay of Benoxaprofen in Plasma

Abstract

A rapid high-performance liquid chromatographic assay for the determination of the anti-inflammatory drug benoxaprofen in human plasma, is described. Plasma samples of 1.0 ml, to which benoxaprofen, and warfarin as an internal standard, had been added, were extracted with ether under acidic conditions. The samples were analyzed on a MicroPak CN-10 column using 25% acetonitrile in water (pH 2.5 with phosphoric acid). Detection was made on a variable wavelength UV absorbance detector at 309 nm.

Samples containing 0.5–10 μg benoxaprofen gave a mean extraction recovery from control plasma of 90.6 ± 6.8% (n=18). Stability tests have shown that benoxaprofen in plasma is stable for at least two weeks after freezing.     

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％。     

High Performance Liquid Chromatographic Determination of Pentamidine in Plasma

Abstract

A high performance liquid chromatographic method for quantitating pentamidine in plasma has been developed. Sample clean-up involved precipitating plasma with acetonitrile containing the internal standard, hexamidine. The supernatant was passed through a C₈ Bond Elut column and eluted with a methanolic solution of sodium 1-heptanesulfonate. The eluate was then analyzed on an Altex C₈ column with a mobile phase consisting of 45% CH₈CN, 0.02% detramethylammonium chloride and 0.1% H₃PO₄. Using fluorescence detection (EX: 275 nm and EM: 340 nm), the detection limit was 1.25 ng/ml for 0.5 ml of plasma. The coefficients of variation for interday and intraday were around 10%.     

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）。     

High Performance Liquid Chromatographic Separation of Bacitracin Methylenedisalicylate

Abstract

Our previously described isocratic RP HPLC procedure was convenient for monitoring and quality control of bacitracin production and Zn - bacitracin feed grade preparations. Separation and quantitative determination of the main active bacitracin components (A₁ B₁ and B₂) are possible and those elution is not interrupted by other ingredients in this type of samples. But when the methylenedisalicylic salt of bacitracin was tested some modification of method were necessary for the correct separation of bacitracin components. Mobile phase had to be modified and polystyrene based packing was an alternative and useful complement to octadecylated silica gel packings.