Application of Reverse Phase Ion-Pair Partition Chromatography to Drugs of Forensic Interest

1977 ◽  
Vol 60 (5) ◽  
pp. 1035-1040 ◽  
Author(s):  
Ira Lurie
Keyword(s):  
Ion Chromatography ◽  
Mobile Phase ◽  
Ergot Alkaloids ◽  
Ion Pair ◽  
Partition Chromatography ◽  
Reverse Phase ◽  
Opium Alkaloids ◽  
Ultraviolet Detector ◽  
Wide Range ◽  
Abused Drugs

Abstract A method is described for determining a wide range of abused drugs by using 1 column, a single isocratic system, and a fixed wavelength (254 nm) ultraviolet detector. Paired-ion chromatography is performed on a reverse phase μBondapak C18 column. Acidic, basic, and neutral drugs, including their corresponding salts, can be determined without prior cleanup. A counter ion, 1-heptane sulfonate, is dissolved in the aqueous organic mobile phase to give a final pH of approximately 3.5. This technique is applicable to ergot alkaloids, phenylethylamines, opium alkaloids, local anesthetics, barbiturates, and other drugs of forensic interest. Five major opium alkaloids in gum opium, namely, morphine, codeine, thebaine, narcotine, and papaverine, can be separated in approximately 20 min.

Determination of Neomycin in Animal Tissues, Using Ion-Pair Liquid Chromatography with Fluorometric Detection

1985 ◽  
Vol 68 (1) ◽  
pp. 29-36
Author(s):  
Badar Shaikh ◽  
Edward H Allen ◽  
John C Gridley
Keyword(s):  
Mobile Phase ◽  
Potassium Phosphate ◽  
Internal Standard ◽  
Ion Pair ◽  
Fluorometric Detection ◽  
Animal Tissues ◽  
Potassium Phosphate Buffer ◽  
Reverse Phase ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method is described for the determination of neomycin in animal tissues. Tissues are homogenized in 0.2M potassium phosphate buffer (pH 8.0); the homogenate is centrifuged, and the supernate is heated to precipitate the protein. The heat-deproteinated extract is acidified to pH 3.5-4 and directly analyzed by LC. The LC method consists of an ion-pairing mobile phase, a reverse phase ODS column, post-column derivatization with o-phthalaldehyde reagent, and fluorometric detection. The LC method uses paromomycin as an internal standard, and separates neomycin from streptomycin or dihydrostreptomycin because they have different retention times. The LC column separates neomycin in 25 min; the detection limit is about 3.5 ng neomycin. The overall recovery of neomycin from kidney tissues spiked at 1-30 ppm was 96% with a 9.0% coefficient of variation. The method was also applied to muscle tissue.

scholarly journals Development and Validation of Simple, Rapid and Sensitive High- Performance Liquid Chromatographic Method for the Determination of Butenafine Hydrochloride

2020 ◽  
pp. 116-125
Author(s):  
Mohammad Javed Ansari ◽  
Mohammed Muqtader Ahmed ◽  
Md. Khalid Anwer ◽  
Mohammed F. Aldawsari ◽  
Saad M. Al Shahrani ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Least Square ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Relative Standard ◽  
Wide Range

Aims: The current paper reports a simple, rapid, sensitive, accurate, and precise Reverse-phase high performance liquid chromatography (RP-HPLC) method with wide range of estimation to determine butenafine hydrochloride in nanosponges. This method has been validated as per ICH norms. Study Design:  Experimental design with influence of variables such as mobile phase composition, flow rate, temperature and wavelength on the chromatographic peaks. Place and Duration of Study: Department of Pharmaceutics, College of Pharmacy, Prince Sattam Bin Abdulaziz University, Al-Kharj, Saudi Arabia between Jan 2020 and March 2020. Methodology: Separation was achieved by utilizing the most commonly used reverse phase column (C-18, 5 μm, 150 mm x 4.6 mm) set at 30ºC and quantified by UV detection at 280 nm after isocratic elution from a mobile phase (70:30 v/v of methanol: phosphate buffer pH 3.0) flowing at 1 ml/min. Results: A sharp and symmetrical peak was observed at 4.08 ± 0.01 minutes. The low variation in peak area and retention time (1.12% and 0.29%, respectively) and a high number of theoretical plates (>2000) indicated this method’s efficiency and suitability. The least square linear regression analysis (Y = 9265.5 X + 1961.4) showed excellent correlation (r2 = 0.999 ± 0.0003) between concentration and peak area of butenafine hydrochloride through a wide concentration range of 1–50 µg/ml. The limits of detection and quantification (LOD and LOQ) were 0.18 µg/ml and 0.57 µg/ml, respectively. The assay or determinations were accurate, precise and reproducible with mean accuracy and mean relative standard deviation of precision of 101.53 ± 0.43% and 0.51 ± 0.11% respectively. Conclusion: The developed RP-HPLC method was simple, sensitive, reproducible with wide range of estimation of butenafine hydrochloride in the nanosponges. The proposed method could be used for the analysis of butenafine hydrochloride in the conventional pharmaceutical formulations such as tablets, syrup, creams including novel formulations such as nanoparticles, nanosponges, nanoemulsions. The proposed method overcomes the specificity, sensitivity and reproducibility related issues of ultraviolet-visible spectroscopy.

Development, Validation and Application of HPLC Method for Metformin in Rabbit Plasma

2019 ◽  
Vol 15 (6) ◽  
pp. 574-579
Author(s):  
Muhammad Ubaid ◽  
Mahmood Ahmad ◽  
Farhan Ahmad Khan ◽  
Ghulam Murtaza
Keyword(s):  
Flow Rate ◽  
Present Method ◽  
Mobile Phase ◽  
Hplc Method ◽  
Plasma Samples ◽  
Rabbit Plasma ◽  
Uv Detector ◽  
Reverse Phase ◽  
T Values ◽  
Pharmacokinetic Evaluation

Objective:This study was aimed at conducting a pharmacokinetic evaluation of metformin in rabbit plasma samples using rapid and sensitive HPLC method and UV detection.Methods:Acetonitrile was used for protein precipitation in the preparation of plasma samples. Reverse phase chromatography technique with silica gel column (250 mm × 4.6 mm, 5 μm) at 30°was used for the separation purpose. Methanol and phosphate buffer (pH 3.2) mixture was used as a mobile phase with flow rate 0.8 ml/min. The wavelength of UV detector was adjusted at 240 nm.Results:The calibration curve was linear in a range of 0.1-1 µg/ml with R² = 0.9982. The precision (RSD, %) values were less than 2%, whereas, accuracy of method was higher than 92.37 %. The percentage recovery values ranged between 90.14 % and 94.97 %. LOD and LOQ values were 25 ng/ml and 60 ng/ml, respectively. Cmax and AUC0-t values were found to be 1154.67 ± 243.37 ng/ml and 7281.83 ± 210.84 ng/ml.h, respectively after treating rabbits with a formulation containing 250 mg metformin.Conclusion:Based on the above findings, it can be concluded that present method is simple, precise, rapid, accurate and specific and thus, can be efficiently used for the pharmacokinetic study of metformin.

scholarly journals Gradient HPLC in the determination of drug lipophilicity and acidity

2001 ◽  
Vol 73 (9) ◽  
pp. 1465-1475 ◽  
Author(s):  
Roman Kaliszan ◽  
Piotr Haber ◽  
Tomasz Baczek ◽  
Danuta Siluk
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Standard Procedure ◽  
Gradient Elution ◽  
Log P ◽  
Retention Data ◽  
Organic Modifier ◽  
Wide Range ◽  
Aqueous Component ◽  
Initial Ph

The linear-solvent strength (LSS) model of gradient elution in high-performance liquid chromatography (HPLC) has been demonstrated to provide parameters of lipophilicity and acidity of analytes. pKa and log kw values are determined in three gradient runs. The first two experiments use an aqueous buffered eluent with a wide-range organic modifier gradient at pH of buffer, providing suppression of ionization of the analyte. That experiment allows an estimate of contents of the organic modifier in the mobile phase (%B), producing requested retention coefficient, k, for the nonionized form of the analyte. The next experiment is carried out with the latter %B and a pH-gradient of the aqueous component of the eluent that is sufficient to overlap possible pKa value of the analyte. The initial pH of the buffer used to make the mobile phase is selected to insure that the analyte is in nonionized form. The resulting retention time allows an estimate of pKa in a solvent of the given %B.The log kw parameter obtained correlated well with the corresponding value obtained by the standard procedure of extrapolation of retention data determined in a series of isocratic measurements. The correlation between log kw and the reference parameter of lipophilicity, log P, was very good for a series of test analytes. The values of pKa were found to correlate with the literature pKa data determined in water for a set of aniline derivatives studied.

Developments in mycotoxin analysis: an update for 2012-2013

2014 ◽  
Vol 7 (1) ◽  
pp. 3-33 ◽  
Author(s):  
F. Berthiller ◽  
P.A. Burdaspal ◽  
C. Crews ◽  
M.H. Iha ◽  
R. Krska ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Ergot Alkaloids ◽  
Tandem Mass ◽  
Wide Range ◽  
Rapid Spread ◽  
Food And Feed ◽  
Mycotoxin Analysis ◽  
The Individual

This review highlights developments in mycotoxin analysis and sampling over a period between mid-2012 and mid-2013. It covers the major mycotoxins: aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxins, patulin, trichothecenes and zearalenone. A wide range of analytical methods for mycotoxin determination in food and feed were developed last year, in particular immunochemical methods and liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS)-based methods. After a section on sampling and sample preparation, due to the rapid spread and developments in the field of LC-MS/MS multimycotoxin methods, a separate section has been devoted to this area of research. It is followed by a section on mycotoxins in botanicals and spices, before continuing with the format of previous reviews in this series with dedicated sections on method developments for the individual mycotoxins.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

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