scholarly journals Separation and Analysis of Aspirin and Metformin HCl Using Green Subcritical Water Chromatography

Molecules ◽  
2018 ◽  
Vol 23 (9) ◽  
pp. 2258 ◽  
Author(s):  
Ninad Doctor ◽  
Yu Yang
Keyword(s):  
Organic Solvents ◽  
High Performance ◽  
Subcritical Water ◽  
Antidiabetic Drug ◽  
Chromatographic Separations ◽  
Pharmaceutical Ingredients ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Subcritical Water Chromatography ◽  
Metformin Hcl

Organic solvents are widely used in pharmaceutical and chemical industry for chromatographic separations. In recent years, subcritical water chromatography (SBWC) has shown ability in replacing hazardous organic solvents used in traditional high-performance liquid chromatography (HPLC). In this work, a pain killer—aspirin—and an antidiabetic drug—metformin HCl—were successfully separated on an XBridge C18 column using no organic solvents in the subcritical water chromatography mobile phase. Both traditional HPLC and subcritical water chromatography were used for comparison purposes. SBWC separation of metformin HCl and aspirin were achieved at 95 °C and 125 °C, respectively. The recovery for both active pharmaceutical ingredients (APIs) obtained by SBWC is 99% in comparing with the stated content of each drug. The relative standard deviation is less than 1% for SBWC assays developed in this work. This level of accuracy and precision achieved by SBWC is the same as that resulted by the traditional HPLC analysis.

scholarly journals COMPARISON OF THREE EXTRACTION METHODS OF ALLOPURINOL IN URIC ACID HERBAL MEDICINE WITH HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY QUANTIFICATION

2021 ◽  
pp. 141-147
Author(s):  
RIMADANI PRATIWI ◽  
RASPATI D. MULYANINGSIH ◽  
NYI M. SAPTARINI
Keyword(s):  
Herbal Medicine ◽  
High Performance ◽  
Solid Phase ◽  
Extraction Methods ◽  
Liquid Extraction ◽  
Filtering Method ◽  
Liquid Liquid Extraction ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Parameters Of Accuracy

Objective: This study was aimed to understand and determine the effectiveness of allopurinol extraction in herbal medicine from three extraction methods based on parameters of accuracy and precision. Methods: The study consisted of three methods including dissolving and filtering, liquid-liquid extraction, and solid-phase extraction with mixed-mode cation exchanger (SPE-MCX). The procedures were carried out using NaOH and HCl in dissolving and filtering method; methanol, HCl, and ethyl acetate in liquid-liquid extraction; and NH4OH elution solvent in SPE-MCX. Results: The results showed that extraction effectiveness based on accuracy level was the dissolving and filtering method>SPE-MCX>liquid-liquid extraction with % recovery+SD of 91.314+2.903%, 87.533+4.950%, and 54.549+3.517%, respectively. The precision level was the dissolution and filtering method>SPE-MCX>liquid-liquid extraction based on % relative standard deviations (RSD) of 3.18%, 5.226%, and 6.446%, respectively. Conclusion: It can be concluded that the allopurinol extraction method with the highest effectiveness based on accuracy and precision parameters in herbal medicine is the dissolving and filtering method.

scholarly journals Column High-Performance Liquid Chromatographic Determination of Norfloxacin and Its Main Impurities in Pharmaceuticals

2008 ◽  
Vol 91 (2) ◽  
pp. 332-338 ◽  
Author(s):  
Branislava Mielji ◽  
Gordana Popovi ◽  
Danica Agbaba ◽  
Slavko Markovi ◽  
Breda Simonovska ◽  
...  
Keyword(s):  
High Performance ◽  
Raw Materials ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Array Detector ◽  
Chromatographic Separations ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A gradient reversed-phase column high-performance liquid chromatographic method was developed for the detection and quantification of norfloxacin and its major impurities in norfloxacin-containing pharmaceuticals. Chromatographic separations were performed under the following experimental conditions: column, Zorbax SB RP-18 (5 m, 250 4.6 mm); injection volume, 20 L; mobile phase, 0.05 M NaH2PO4 (pH 2.5)acetonitrile (87 + 13) for 16 min and (58 + 42) for 9 min (stepwise gradient); and flow rate, 1.3 mL/min. All analyses were performed at 25C, and the eluate was monitored at 275 nm using a diode array detector. Linearity (correlation coefficient = 0.999), recovery (99.3101.8), relative standard deviation (0.20.7), and quantitation limit (0.120.47 g/mL) were evaluated and found to be satisfactory. The method is simple, rapid, and convenient for purity control of norfloxacin in both raw materials and dosage forms.

scholarly journals Determination of Active Vitamin B12 (Cobalamin) in Dietary Supplements and Ingredients by Reversed-phase Liquid Chromatography (P13-040-19)

2019 ◽  
Vol 3 (Supplement_1) ◽  
Author(s):  
Hong You
Keyword(s):  
Liquid Chromatography ◽  
Vitamin B12 ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Funding Sources ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Analysis Center ◽  
Micronutrient Malnutrition

Abstract Objectives Vitamin B12 dietary supplement can be critical to the alleviation strategies against micronutrient malnutrition and food insecurity. A high-performance liquid chromatography with ultraviolet detection (HPLC-UV) method has been developed and validated, for the quantitation of four bioactive forms of vitamin B12 (adenosylcobalamin, cyanocobalamin, hydroxocobalamin, methylcobalamin) from dietary ingredients and supplements. Methods A Plackett-Burman factorial study was used to identify factors that contributed to the extraction of cobalamins. Significant factors were selected to produce the improved HPLC method for cobalamin separation. This method was then subjected to a single-laboratory validation according to the AOAC International guidelines for linearity, suitability, detection limits, accuracy, and precision. Results The method achieves chromatographic baseline resolution of vitamin B12 forms on a modern column platform without the expensive requirement of an ultra-high pressure liquid chromatography and/or mass spectrometry. The method has a wide analytical range (0.0005% w/w - 85% w/w), high precision (repeatability relative standard deviations ranged from 1.08% to 3.06%), and high accuracy (>96% spike recovery rate). The method detection and quantification limits are less than 0.16 and 0.52 µg/mL, respectively. Conclusions To our best knowledge, the method is simpler, less time-consuming, and more economical than other published methods for its intended uses. Funding Sources Eurofins Supplement Analysis Center, Eurofins Scientific, Inc. MilliporeSigma Supporting Tables, Images and/or Graphs

Ultra-trace Extraction of Two Bactericides Via Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction

2020 ◽  
Author(s):  
Xun Gao ◽  
Xinxin Si ◽  
Yunxia Yuan ◽  
Kexin Chen ◽  
Kunming Qin
Keyword(s):  
High Performance ◽  
Optimum Conditions ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Ultrasound Assisted ◽  
Ultra Trace ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

Abstract Background A simple, rapid and sensitive method coupling ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) with ultra-high performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous determination of malachite green (MG) and crystal violet (CV) in different water samples. Objective In ultrasound-assisted DLLME procedure, several parameters affecting the extraction efficiency, including pH, type and volume of the extraction and dispersive solvents, extraction time, ionic strength, were optimized to improve the accuracy and precision of this method. Methods MG and CV were extracted and preconcentrated using dichloromethane and acetonitrile as the extraction and dispersive solvents, respectively. Results Under the optimum conditions, the proposed method affords good linearity in the range of 0.40–20.0 ng/L, and the limit of detections were 0.21 and 0.32 ng/L for MG and CV, respectively. The recoveries of the method at three spiked levels were in the range of 83.4–94.2% with relative standard deviations lower than 4.7% (n = 3). Conclusions Satisfactorily, no significant matrix effect has been found as the data ranged between 68% and 102%.

Determination of patulin and hydroxymethylfurfural in beverages by UPLC-PDA

2020 ◽  
pp. 1-8
Author(s):  
M. Pernica ◽  
J. Martiník ◽  
R. Boško ◽  
V. Zušťáková ◽  
K. Benešová ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Penicillium Expansum ◽  
Limit Of Quantification ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Validation Parameters ◽  
Photodiode Array ◽  
Quantification Accuracy

The present study describes using molecularly imprinted polymer (MIP) technology for determination of patulin (PAT) and 5-hydroxymethylfurfural (5-HMF) in beverages by ultra-high performance liquid chromatography coupled to photodiode array (UPLC-PDA). PAT (4-hydroxy-4H-furo[3,2-c]pyran-2(6H)-one) is a mycotoxin produced by Penicillium fungi and Penicillium expansum is probably the most commonly encountered species that infects apples during their growth, harvest, storage or processing. The occurrence of PAT as a natural contaminant of apples is a worldwide problem. 5-HMF (also known as 5-(hydroxymethyl) furan-2-carbaldehyde), is formed in the Maillard reaction as well as during caramelisation. It is a good storage time-temperature marker and flavour indicator, especially in beverages such as wine, beer, but also cider and apple juice which may contain PAT. PAT and 5-HMF were separated within 2 min using a Luna Omega C18 column and the PDA detector wavelength was set to 276 nm. The validation parameters of the analytical method such as linearity, limit of detection, limit of quantification, accuracy and precision were tested. The calibration curves were linear at least in the range 50-1000 ng/ml with a good linearity (R2>0.999) for both analytes, the limit of detection and the limit of quantification for PAT and 5-HMF were in the range 4.9-6.6 and 16.1-21.8 μg/l, respectively. The recoveries of the selected analyte were in the range 61.9-109.0% with a precision of <8.2% (relative standard deviation (RSD)) for PAT and in the range 50.8-98.0% with a precision of <10.0% (RSD) for 5-HMF. The validated procedure was successfully applied for the analysis of PAT and 5-HMF in beverages from retail shops.

Validation of the SafTest Percent Fat for the Measurement of the Fat Content of Meat Meals, Fish Meal, and Potato Chips, Crackers, and Other and Grain-Based Snack Products: AOAC Performance Tested Method  SM #082004

2020 ◽  
Author(s):  
Virginia C Gordon ◽  
Christopher C Rainey ◽  
Willainia C Studmire
Keyword(s):  
Organic Solvents ◽  
Membrane Separation ◽  
Standard Procedure ◽  
Fat Content ◽  
Study Objective ◽  
Independent Laboratory ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Snack Products ◽  
Stability And Consistency

Abstract Background The Official American Oil Chemists Society (AOCS) Standard Procedure Aa 4–38, AOCS Standard Procedure Am 5–04, ISO 11085:2015, and similar methods are based on extraction of fats from food products using organic solvents. These methods require large volumes of organic solvents and up to 18-hour extractions. The SafTest Percent Fat measures fat content as “total triglycerides” in solubilized snack products and meals using micro-analytical and membrane separation principles. Objective The study objective is to validate the SafTest Percent Fat in an internal study and an independent laboratory study. Method Comparability to AOCS Standard Procedure Aa 4–38 or AOCS Standard Procedure Am 5–04, LOQ, selectivity, robustness, stability, and consistency were determined. Results Mean recoveries from replicate analyses of SafTest control samples at three concentrations yielded 101 to 103%. The relative standard deviations of repeatability (RSDr) were below 5%. Studies of meat meals and snacks analyzed using the SafTest Percent Fat demonstrated RSDr of 2.3 to 5.6% compared to 2.6 to 4.9% for AOCS Aa 4–38. The method demonstrated average recoveries ranging from 88.8 to 116.2% compared to the AOCS methods results performed in two contract laboratory studies and an independent laboratory validation. Conclusions The SafTest Percent Fat test can determine fat content in meals and snack matrices with accuracy and precision comparable to results from AOCS Aa 4–38 and AOCS Am 5–04. Highlights The SafTest Percent Fat test uses small reagent volumes, instrumental analysis, easy-to-use standardized procedures, and rapid analysis times for fat content determination.

scholarly journals A novel analytical approach for reducing the consumption of organic solvents in the charge transfer-based spectrophotometric analysis: Application in the analysis of certain antihypertensive drugs

2010 ◽  
Vol 60 (4) ◽  
pp. 493-501 ◽  
Author(s):  
Ibrahim Darwish ◽  
Ashraf Mahmoud ◽  
Abdul-Rahman Al-Majed
Keyword(s):  
Charge Transfer ◽  
Organic Solvents ◽  
Analytical Approach ◽  
Antihypertensive Drugs ◽  
Spectrophotometric Analysis ◽  
Optimum Conditions ◽  
Pharmaceutical Dosage Forms ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Analysis Application

A novel analytical approach for reducing the consumption of organic solvents in the charge transfer-based spectrophotometric analysis: Application in the analysis of certain antihypertensive drugsThe present study describes the development of a novel analytical approach that can reduce by 50-fold the consumption of organic solvents in the charge transfer (CT)-based spectrophotometric analysis. The proposed approach employed 96-microwell assay plates for carrying out the reaction. The CT reaction between the electron-donating analyte and electron-accepting reagent was performed in microwells (200-μL of organic solvent) and the color signals were measured with a microwell-plate reader. Optimum conditions for the proposed approach were established for two antihypertensive drugs, namely ramipril (RML) and lisinopril (LSL) as model compounds for the electron-donating analytes, and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) as a π-electron acceptor. Under the optimum conditions, Beer's law was obeyed in the concentration range of 6-100 and 6-60 μg mL-1for RML and LSL, respectively. The limits of detection were 0.97 and 1.10 μg mL-1for RML and LSL, respectively. The precision of the methods was satisfactory; the values of relative standard deviations did not exceed 1.1 %. The proposed approach was successfully applied to the analysis of pharmaceutical dosage forms with good accuracy and precision. The results were comparable with those of the reported methods. The approach described herein is of great practical value in pharmaceutical analysis because it reduces the exposure of analysts to the toxic effects of organic solvents, lowers the analysis cost by 50-fold, and it has a high throughput property. Although the approach was validated for RML and LSL, the same methodology could be used for any electron-donating analyte for which a CT-reaction can be performed.

Reversed-Phase High Performance Liquid Chromatographic Analysis of Three First Line Anti-Tuberculosis Drugs

2019 ◽  
Vol 69 (12) ◽  
pp. 3590-3592
Author(s):  
Nela Bibire ◽  
Romeo Iulian Olariu ◽  
Luminita Agoroaei ◽  
Madalina Vieriu ◽  
Alina Diana Panainte ◽  
...  
Keyword(s):  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
First Line ◽  
Pharmaceutical Ingredients ◽  
Liquid Chromatographic

Active pharmaceutical ingredients such as isoniazid, pyrazinamide and rifampicin are among the most important first-line anti-tuberculosis drugs. A simple, rapid and sensitive reversed phase-high performance liquid chromatographic assay method for the simultaneous determination of isoniazid, pyrazinamide and rifampicin has been developed. Separation of the interest compounds was achieved in a 10 min chromatographic run in gradient elution mode on a Zorbax SB-C18 stainless steel column (150 � 4 mm, 5 mm) using a guard column containing the same stationary phase. The gradient elution was carried out with a mobile phase of 10% CH3CN aqueous solution for channel A and 50% CH3CN in pH = 6.8 phosphate buffer (20 mM), to which 1.5 mL triethylamine were added for channel B. Quantification of the analyzed substances was carried out spectrophotometrically at 269 nm. Detection limits of 0.48 mg/L for isoniazid, 0.52 mg/L for pyrazinamide and 0.48 mg/L for rifampicin were established for the developed assay method. The present work showed that the proposed analysis method was advantageous for simple and rapid analysis of the active pharmaceutical ingredients in pharmaceuticals and biological fluids.

Determination of Selected Phthalates in Some Commercial Cosmetic Products by HPLC-UV

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural
Keyword(s):  
High Performance ◽  
Phthalate Esters ◽  
High Sensitivity ◽  
Hplc Method ◽  
Cosmetic Products ◽  
Limit Of Quantification ◽  
Nail Polish ◽  
Accuracy And Precision ◽  
Butyl Phthalate

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.

Sign in / Sign up

Export Citation Format

Share Document