scholarly journals Determination of Sulfonamides in Feeds by High-Performance Liquid Chromatography after Fluorescamine Precolumn Derivatization

Molecules ◽  
2019 ◽  
Vol 24 (3) ◽  
pp. 452 ◽  
Author(s):  
Ewelina Patyra ◽  
Monika Przeniosło-Siwczyńska ◽  
Krzysztof Kwiatek
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Phase System ◽  
Precolumn Derivatization ◽  
Detection Capability ◽  
Limit Of Quantification ◽  
Decision Limit ◽  
Limit Detection

A new multi-residue method for the analysis of sulfonamides (sulfadiazine, sulfamerazine, sulfamethazine, sulfaguanidine and sulfamethoxazole) in non-target feeds using high-performance liquid chromatography-fluorescence detection (HPLC-FLD) and precolumnderivatization was developed and validated. Sulfonamides (SAs) were extracted from feed with an ethyl acetate/methanol/acetonitrile mixture. Clean-up was performed on a Strata-SCX cartridge. The HPLC separation was performed on a Zorbax Eclipse XDB C18 column with a gradient mobile phase system of acetic acid, methanol, and acetonitrile. The method was validated according to EU requirements (Commission Decision 2002/657/EC). Linearity, decision limit, detection capability, detection and quantification limits, recovery, precision, and selectivity were determined, and adequate results were obtained. Using the HPLC-FLD method, recoveries were satisfactory (79.3–114.0%), with repeatability and reproducibility in the range of 2.7–9.1% to 5.9–14.9%, respectively. Decision limit (CCα) and detection capability (CCβ) were 197.7–274.6 and 263.2–337.9 µg/kg, respectively, and limit of detection (LOD) and limit of quantification (LOQ) were 34.5–79.5 and 41.3–89.9 µg/kg, respectively, depending on the analyte. Results showed that this analytical procedure is simple, rapid, sensitive, and suitable for the routine control of feeds.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

scholarly journals ESTIMATION OF GUGGULSTERONE-Z IN GOKSHURADI GUGGULU USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 (11) ◽  
pp. 204
Author(s):  
Kanan G Gamit ◽  
Niraj Y Vyas ◽  
Nishit D Patel ◽  
Manan A Raval
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Photodiode Array Detector ◽  
Validation Parameters ◽  
Photodiode Array

Objective: A study was aimed to estimate guggulsterone-Z (GZ) in Gokshuradi Guggulu (GG).Methods: An analytical method was developed and validated using Waters Alliance high-performance liquid chromatography system (Empower software), equipped with photodiode array detector. Separation was achieved using Phenomenex, C-18 (250 mm×4.6 mm, 5 μ) column. Mobile phase consisted of acetonitrile:water (70:30,v/v). Flow rate was set to 1 ml/min and detection was performed at 251 nm.Results and Discussion: Validation parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were performed. Amount of GZ was estimated using linearity equation.Conclusion: GG was found to contain 0.815±0.03 g% w/w GZ. Validated method may be used as one of the parameters to standardize the formulation.

scholarly journals Estimation of Abamectin Residues Present in Tea: High-Performance Liquid Chromatography Technique

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Madasamy Kottiappan ◽  
Shanmugaselvan Veilumuthu Anandhan ◽  
Selvaganapathi Chandran
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Black Tea ◽  
Water Mixture ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Acetone Water ◽  
Sensitive Method

A simple, reliable, and sensitive method was based on high-performance liquid chromatography (HPLC) was developed and validated for the estimation of abamectin residues present in tea. The abamectin residues extracted with acetone-water mixture (70 : 30, v/v) and derivatised with 1-methylimidazole (1-MIM) and trifluoroacetic anhydride (TFAA) were estimated by HPLC using fluorescence detector (FLD). The technique was validated in terms of linearity, precision, recovery, specificity, limit of detection (LOD), and limit of quantification (LOQ). A good linear relationship () was absorbed in the abamectin concentration range from 0.01 to 1.0 μg mL−1. The limit of detection and limit of quantification of the method were 0.01 and 0.02 μg g−1, respectively. The average recoveries of the pesticide from black tea and dried green leaves ranged from 83.3 to 103.8% and 83.8 to 98.0%, respectively.

scholarly journals Validation of a Reversed-Phase High Performance Liquid Chromatography Method for the Simultaneous Analysis of Cysteine and Reduced Glutathione in Mouse Organs

2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Serena Brundu ◽  
Lucia Nencioni ◽  
Ignacio Celestino ◽  
Paolo Coluccio ◽  
Anna Teresa Palamara ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reduced Glutathione ◽  
Reversed Phase ◽  
Mouse Strains ◽  
Precolumn Derivatization ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Validation Parameters

A depletion of reduced glutathione (GSH) has been observed in pathological conditions and in aging. Measuring GSH in tissues using mouse models is an excellent way to assess GSH depletion and the potential therapeutic efficacy of drugs used to maintain and/or restore cellular redox potential. A high performance liquid chromatography (HPLC) method for the simultaneous determination of GSH and cysteine (Cys) in mouse organs was validated according to USA and European standards. The method was based on separation coupled with ultraviolet detection and precolumn derivatization with 5,5′-dithiobis-(2-nitrobenzoic acid) (DTNB). The required validation parameters, that are, selectivity, linearity, lower limit of quantification, precision, accuracy, recovery, and stability, were studied for spleen, lymph nodes, pancreas, and brain. The results showed that the lower limits of quantification were 0.313 μM and 1.25 μM for Cys and GSH, respectively. Intraday and interday precisions were less than 11% and 14%, respectively, for both compounds. The mean extraction recoveries of Cys and GSH from all organs were more than 93% and 86%, respectively. Moreover, the stability of both analytes during sample preparation and storage was demonstrated. The method was accurate, reliable, consistent, and reproducible and it was useful to determine Cys and GSH in the organs of different mouse strains.

scholarly journals A microemulsion high-performance liquid chromatography (MELC) method for the separation and determination of hydrolyzed tenuifolin in Radix Polygalae

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Hui Yan ◽  
Zhuan-Di Zheng ◽  
Hong-Fei Wu ◽  
Xiao-Chuang Liu ◽  
An Zhou
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Limit Of Quantification ◽  
Analyte Molecule ◽  
Oil In Water

AbstractTenuifolin was used as a reliable chemical marker for the quality control of Radix Polygalae. The determination of tenuifolin is challenging because the analyte molecule lacks a suitable chromophore. The aim of this study was to establish a microemulsion high-performance liquid chromatography (MELC) method which is robust and sensitive, and can separate and determine tenuifolin in Radix Polygalae using an oil-in-water (O/W) microemulsion mobile phase. The separations were performed on a C18 (4.6 × 250 mm, 5 μm) column at 25 °C using a flow rate of 1.0 mL/min, and an ultraviolet detection wavelength of 210 nm. The microemulsion mobile phase comprised 2.8% (w/v) sodium dodecyl sulfate (SDS), 7.0% (v/v) n-butanol, 0.8% (v/v) n-octane and 0.1% (v/v) aqueous orthophosphate buffer (H3PO4). The linearity analysis of tenuifolin showed a correlation coefficient of 0.9923 in the concentration range of 48.00–960.00 µg/mL. The accuracy of the method based on three concentration levels ranged from 96.23% to 99.28%; the limit of detection (LOD) was 2.34 µg/mL, and the limit of quantification (LOQ) was 6.76 µg/mL. The results of our study indicated that the optimized MELC method was sensitive and robust, and can be widely applied for the separation and determination of tenuifolin in Radix Polygalae.

scholarly journals Extraction and Determination of Oxymatrine Pesticide in Environmental Sample and in its Formulation using High-Performance Liquid Chromatography

2020 ◽  
Vol 8 (2) ◽  
pp. 1-7
Author(s):  
Ihsan M. Shaheed ◽  
Saadiyah A. Dhahir
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction

The quinolizindine alkaloid compound, oxymatrine pesticide, was analysis in the river water samples collected from different agriculture areas in the Iraqi city of Kerbala and also in its formulation using developed reverse-phase high-performance liquid chromatography method. Acetonitrile:methanol (60:40 v/v) was chosen as mobile phase at pH (7.0), flow rate 0.5 mL/min, and 20 µL as volume injection. Modified ecological-friendly method, dispersive liquid-liquid microextraction, was used for the extraction of oxymatrine from water samples. Linearity study was constructed from 0.1 to 70 μg/mL at λmax 205 nm. The limit of detection and limit of quantification were 0.025 and 0.082 μg/mL, respectively, and the relative standard deviation (RSD) % was 0.518%. Three spiked levels of concentration (20.0, 40.0, and 70.0 μg/mL) were used for the validation method. The percentage recovery for the three spiked samples was ranged between 98.743 and 99.432 and the RSD% was between 0.051 and 0.202%, the formulation studies of oxymatrine between 99.487 and 99.798, and the RSD% was ranged from 0.045 to 0.057%. The developed method can be used accurately and selectively for the determination of oxymatrine in environmental samples and in the formulation.

scholarly journals Development and Validation of a High-Performance Liquid Chromatography Method for Quality Assessment of Oriental Medicine, Dokhwalgisaeng-Tang

2021 ◽  
Vol 11 (17) ◽  
pp. 7829
Author(s):  
Chang-Seob Seo ◽  
Hyeun-Kyoo Shin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Herbal Medicine ◽  
Formic Acid ◽  
Quality Assessment ◽  
High Performance ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Chromatography Method

Dokhwalgisaeng-tang (DHGST) is an herbal medicine formula that is frequently used in the treatment of arthritis in Korea and consists of 16 medicinal herbs. In this study, a simultaneous analysis method for quality assessment of DHGST by universal and widely used high-performance liquid chromatography was developed and validated. Twenty-four marker components were separated on a reverse-phase SunFire C18 column (4.6 × 250 mm, particle size; 5 μm) maintained at 40 °C using a gradient elution of two mobile phase systems (0.1% aqueous formic acid and 0.1% formic acid in acetonitrile). The developed method was validated via linearity, limit of detection, limit of quantification, recovery, and precision. Using the developed method, 24 marker components in DHGST were founded at 0.23–14.68 mg/g, and this method will be used as basic data for the quality assessment of DHGST or other herbal medicine prescriptions.

scholarly journals Determination of Aflatoxin B1 in Feedstuffs without Clean-Up Step by High-Performance Liquid Chromatography

2018 ◽  
Vol 2018 ◽  
pp. 1-8 ◽  
Author(s):  
Sasiprapa Choochuay ◽  
Jutamas Phakam ◽  
Prakorn Jala ◽  
Thanapoom Maneeboon ◽  
Natthasit Tansakul
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Precolumn Derivatization ◽  
Broken Rice ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Aflatoxin B

A reliable and rapid method has been developed for the determination of aflatoxin B1 (AFB1) in four kinds of feedstuffs comprising broken rice, peanuts, corn, and fishmeal. A sample preparation was carried out based on the QuEChERS method with the exclusion of the clean-up step. In this study, AFB1 was extracted using acetonitrile/methanol (40/60 v/v), followed by partitioning with sodium chloride and magnesium sulfate. High-performance liquid chromatography with precolumn derivatization and fluorescence detection was performed. The coefficients of determination were greater than 0.9800. Throughout the developed method, the recovery of all feedstuffs achieved a range of 82.50-109.85% with relative standard deviation lower than 11% for all analytes at a concentration of 20-100 ng/g. The limit of detection (LOD) ranged from 0.2 to 1.2 ng/g and limit of quantitation (LOQ) ranged from 0.3 to 1.5 ng/g. The validated method was successfully applied to a total of 120 samples. The occurrence of AFB1 contamination was found at the following concentrations: in broken rice (0.44-2.33ng/g), peanut (3.97-106.26ng/g), corn (0.88-50.29 ng/g), and fishmeal (1.06-10.35 ng/g). These results indicate that the proposed method may be useful for regularly monitoring AFB1 contamination in feedstuffs.

scholarly journals EXTRACTION AND DETERMINATION OF TEBUCONAZOLE IN ENVIRONMENTAL SAMPLES FROM THE CITY OF KERBALA, IRAQ AND IN ITS FORMULATION USING HIGH- PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)

2020 ◽  
Vol 17 (34) ◽  
pp. 1046-1054
Author(s):  
Ihsan Mahdi SHAHEED ◽  
Saadiyah Ahmed DHAHIR
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Percentage Recovery ◽  
Relative Standard

The triazole, tebuconazole pesticide, was determined in its formulation and also in the river water samples collected from different agriculture areas in the Iraqui city of Kerbala using developed high-performance liquid chromatography method(HPLC) with UV-visible detection, The mobile composition phase was a mixture of acetonitrile:methanol (50:50 v/v) and the column was C18 (250 cm x 4.6 mm,5μm). Also modified dispersive liquidliquid microextraction (DLLME), which is regarded as an ecological -friendly method, was used for the extraction of tebuconazole from water samples using acetonitrile and chloroform as solvents extraction and dispersive agent, respectively. Linearity to maintain the calibration curve was achieved from (0.1-70) μg.mL-1 with a limit of detection(0.053) μg.mL-1 and limit of quantification (0.174) μg.mL-1. Three spiked levels of concentration (1.0, 5.0, and 10) μg.mL-1 were used for the validation of the method. The relative standard deviation (RSD%) was (0.294- 0.813)%, and the percentage recovery was (100.001-100.005). The formulation studies for two different concentrations (10 and 40) μg.mL-1, which prepared from tebuconazole formulation (Raxil ODS2 2%), gave acceptable percentage recovery between (98.956-99.833). The developed method can be used accurately for the determination of tebuconazole in water samples and in the formulation of tebuconazole effectively.

scholarly journals CONTENT VARIATIONS OF CARBAMAZEPINE TABLETS IN IRAQI COMMUNITY PHARMACIES: APPLICATION OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ASSAY METHOD

2018 ◽  
Vol 11 (2) ◽  
pp. 117
Author(s):  
Mohanad Naji Sahib
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
High Standard ◽  
Assay Method ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Middle East Countries

 Objective: There is paucity in the literature and documentation regarding the post-marketing product quality in Iraq and Middle East countries in general. Therefore, a simple reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the determination of carbamazepine (CMZ) content in post-marketed tablet dosage form.Methods: The RP-HPLC analysis was run at a flow rate of 1 ml/min with a mixture of methanol: water (70:30) mobile phase using a Thermo Synchronise C18 column at a UV detection wavelength of 230 nm. The method was validated for selectivity, linearity, precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), solution stability, and robustness.Results: The calibration curve was linear over a concentration range of 1–20 μg/ml (r2=0.9999) with LOD and LOQ of 0.01 and 0.04 μg/ml, respectively. The intraday and interday precision and accuracy were between 0.04–1.67% and 0.04–0.78%, respectively. The results of analysis of the four brands of CMZ tablets were passed the European Pharmacopoeia specification but with a high standard deviation of mean drug content of some brands.Conclusion: This study shows that the quality of post-marketed drugs and/or the storage conditions in developing countries must be carefully assessed for a better therapeutic response.

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