scholarly journals Validation of an HPLC-UV method for the identification and quantification of bioactive amines in chicken meat

2016 ◽  
Vol 68 (3) ◽  
pp. 805-813 ◽  
Author(s):  
D.C.S. Assis ◽  
L.D.M. Menezes ◽  
A.L. Lima ◽  
R.W.T. Klein ◽  
L.G.D. Heneine ◽  
...  
Keyword(s):  
Trichloroacetic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Chicken Meat ◽  
Coefficient Of Determination ◽  
Performance Parameters ◽  
Limit Of Quantification ◽  
Ultraviolet Detection ◽  
Ultraviolet Detector

ABSTRACT A high-performance liquid chromatography with ultraviolet detection (HPLC-UV) method was validated for the study of bioactive amines in chicken meat. A gradient elution system with an ultraviolet detector was used after extraction with trichloroacetic acid and pre-column derivatization with dansyl chloride. Putrescine, cadaverine, histamine, tyramine, spermidine, and spermine standards were used for the evaluation of the following performance parameters: selectivity, linearity, precision, recovery, limits of detection, limits of quantification and ruggedness. The results indicated excellent selectivity, separation of all amines, a coefficient of determination greater than 0.99 and recovery from 92.25 to 102.25% at the concentration of 47.2mg.kg-1, with a limit of detection at 0.3mg.kg-1 and a limit of quantification at 0.9mg.kg-1 for all amines, with the exception of histamine, which exhibited the limit of quantification, of 1mg.kg-1. In conclusion, the performance parameters demonstrated adequacy of the method for the detection and quantification of bioactive amines in chicken meat.

scholarly journals Simultaneous Identification and Quantification of Canrenone and 11-α-Hydroxy-Canrenone by LC-MS and HPLC-UVD

2011 ◽  
Vol 2011 ◽  
pp. 1-7 ◽  
Author(s):  
Da-Ming Huang ◽  
Tian-Zhen Zhang ◽  
Feng-Jie Cui ◽  
Wen-Jing Sun ◽  
Li-Ming Zhao ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Elution Time ◽  
Ultraviolet Detector ◽  
Simultaneous Identification ◽  
Identification And Quantification

A procedure for simultaneous identification and quantification of canrenone and its biotransformed product 11-α-hydroxy-canrenone by high-performance liquid chromatography with ultraviolet detector (HPLC-UVD) and mass spectrometry (LC-MS) methods was proposed. The optimal determination variables on the HPLC-UVD or LC-MS coupled with a ZORBAX Eclipse XDB-C18 column (150 mm × 4.6 mm, 5 μm) were set as follows: detection wavelength of 280 nm, mobile phase of water and methanol gradient elution, temperature for the chromatographic column of 30°C, flow rate of mobile phase of 0.8 mL/min, sample injection volume of 5 μL, and elution time of 40 min. The MS conditions were set as follows: the flow rate of sheath gas, aux gas, and sweep gas were kept at 35 arb, 5 arb, and 0 arb, respectively. The temperature of capillary was held at 300°C, and capillary voltage was set at 30.00 V. Tube lens were performed at 100.00 V. The proposed method was validated by linearity ( ≥ 0.9910), average recovery (94.93%, RSD1.21%), precision (RSD ≤ 1.31%), limit of detection, and limit of quantification (LOD 0.1~0.12 mg/L, LOQ 0.5~0.67 mg/L), which proved to be affordable for simultaneously determining canrenone and its bio-transformed product 11-α-hydroxy-canrenone.

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 Pre-Concentration and Determination of Tetracyclines Antibiotics Residues in Water Samples Using RGO/Fe3O4 Nanocomposite as Extraction Sorbent

2021 ◽  
Vol 21 (5) ◽  
pp. 1196
Author(s):  
Ungku Amirul Arif Ungku Abdullah ◽  
Nor Suhaila Mohamad Hanapi ◽  
Wan Nazihah Wan Ibrahim ◽  
Nursyamsyila Mat Hadzir ◽  
Nurzaimah Zaini ◽  
...  
Keyword(s):  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Coefficient Of Determination ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Magnetic Solid

Existing methods used in tracing Tetracyclines' antibiotics (TCAs) residues which pose serious environmental problems, consume high amounts of organic solvents, are time-consuming, and are relatively expensive. A simple and effective magnetic solid-phase extraction (MSPE) based on reduced graphene oxide/magnetite (RGO/Fe3O4) nanocomposite sorbent was successfully developed for preconcentration and extraction of TCAs residues from water samples. The analytes were determined by high-performance liquid chromatography with a diode-array detector (HPLC-DAD). The synthesized nanocomposite was characterized using Fourier-transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD), and field emission scanning electron microscopy (FESEM). Sample pH, amount of adsorbent, sample volume, extraction time, desorption time, and desorption solvent were evaluated and optimized. Under optimized conditions, the method demonstrated good linearity over the concentration range of 0.05–1.0 mg L–1 with the coefficient of determination (R2) ≥ 0.9978. Limit of detection (LOD) and limit of quantification (LOQ) were 0.006–0.011 mg L–1 and 0.019–0.036 mg L–1, respectively. The accuracy and precision of the developed method were proven by good analyte recovery (89.77–106.33%) and acceptable precision with relative standard deviation, RSD ≤ 5.54%. The results showed that magnetic solid RGO/Fe3O4 could be a suitable adsorbent in the preconcentration and extraction of TCAs in water samples.

scholarly journals Monitoring of Aflatoxin B1 in Dry Aged Meats using a modified HPLC-FLD method

2021 ◽  
Vol 26 (4) ◽  
pp. 2885-2891
Author(s):  
HATICE AHU KAHRAMAN ◽  
HIDAYET TUTUN
Keyword(s):  
Aflatoxin B1 ◽  
High Performance ◽  
Limit Of Detection ◽  
Meat Products ◽  
Performance Parameters ◽  
Limit Of Quantification ◽  
Time Saving ◽  
Modified Method ◽  
Meat Samples

The presence of aflatoxins residues in meat and meat products occurs through ingestion of feeds contaminated with Aflatoxin B1 (AFB1) or during the processing of the meat products. Little research has been conducted concerning the detection of AFB1 on meat. The aim of this study was to modify the method for AFB1 determination by high performance liquid chromatography with fluorescence detection in dry aged meats. The aged meat samples used for determination of AFB1 were obtained from a commercial dry aged meat plants and produced for 28 days in a meat plant chiller. All meat samples were analyzed according to the modified method. The samples were cleaned to remove impurities by using a immunoaffinity column. Photochemical reactor was used for the recording and evaluation of the chromatograms. The analytical performance parameters showed that the method was specific for AFB1 detection in the meat samples. Recovery rate, reproducibility (RSDr%) and repeatability (RSDR%) were found to be 85.889%, 3.822% and 6.601%, respectively. Limit of detection and limit of quantification were 0.15 ng/mL and 0.501 ng/mL, respectively. AFB1 was not detected in the meat samples. Our results indicated that the method modified for monitoring AFB1 level in the meats was simple, time-saving and reliable.

scholarly journals Simultaneous determination of some illegal antihypertensive and diuretic drugs in traditional herbal preparations by HPLC-DAD

2021 ◽  
Vol 4 (2) ◽  
pp. 99-108
Author(s):  
Hung Pham Van ◽  
Son Tran Cao ◽  
Kieu Anh Nguyen Thi ◽  
◽  
◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Local Market ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Herbal Products ◽  
Herbal Preparations ◽  
Diuretic Drugs

A simple, stable, and specific high-performance liquid chromatography coupled with a DAD detector (HPLC-DAD) method has been developed and validated for the simultaneous determination of amlodipine, felodipine, furosemide, nifedipine, and spironolactone in traditional herbal products. The analytes were extracted in acetonitrile: water (50 : 50, v/v) with help of the ultrasonic. The separation of analytes was performed in an Apollo C18 column (250 × 4.6 mm; 5 μm) and a mobile phase consisting of mixture acetonitrile: 0.1% phosphoric acid in gradient elution. The analyzed drugs were detected at 238 nm. The method was validated according to the AOAC International guidelines concerning specificity, linearity, precision (repeatability, intermediate precision), accuracy, limit of detection (LOD), and limit of quantification (LOQ). The method can detect the studied drugs at the concentration of 0.66 to 1.25 μg/g for dry samples and 0.10 to 0.24 μg/mL for liquid samples. The method was successfully applied in the analysis of 17 samples in the local market. No samples were found positive for the substances to be analyzed.

Specific and Sensitive Measurement of FK506 and Its Metabolites in Blood and Urine of Liver-Graft Recipients

1992 ◽  
Vol 38 (10) ◽  
pp. 2025-2032 ◽  
Author(s):  
U Christians ◽  
F Braun ◽  
M Schmidt ◽  
N Kosian ◽  
H M Schiebel ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Particle Beam ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Liver Graft ◽  
Limit Of Quantification ◽  
Solid Liquid ◽  
Liquid Chromatographic

Abstract A specific and sensitive assay for quantifying the immunosuppressant FK506 and its metabolites in blood and urine was developed. 32-O-Acetyl FK506 was synthesized and used as internal standard. FK506 and its metabolites were purified from the samples by solid-liquid extraction and were injected into a high-performance liquid chromatographic (HPLC) system linked to a mass spectrometer (MS) by particle-beam interface. The FK506 derivatives were separated from interfering material by use of a 100 x 4 mm C8 analytical column and water/acetonitrile or water/methanol gradient elution; they were detected by negative chemical ionization with methane as reagent gas. The limit of detection was 25 pg in a standard solution, and the limit of quantification in blood was 250 pg (extracted from 1 mL of blood). The CV was 11.3% at 5 ng, and no interferences with other drugs were found.

scholarly journals Development and Validation of an Analytical Method for Determination of Ergot Alkaloids in Animal Feedingstuffs with High Performance Liquid Chromatography-fluorescence Detection

2016 ◽  
Vol 19 (3) ◽  
pp. 559-565 ◽  
Author(s):  
E. Kowalczyk ◽  
E. Patyra ◽  
A. Grelik ◽  
K. Kwiatek
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
High Performance ◽  
Limit Of Detection ◽  
Ergot Alkaloids ◽  
Coefficient Of Determination ◽  
Limit Of Quantification ◽  
Modified Quechers

Abstract A high performance liquid chromatography combined with fluorescence detection (HPLC-FLD) method was developed for determination of five ergot alkaloids (EA): ergometrine, ergotamine, ergocornine, ergocrypine and ergocristine in animal feedingstuffs. The method was based on the application of QuEChERS salts for extraction and modified QuEChERS dispersive SPE for the cleanup step. Alkaloids separation was performed on a C18, 250 mm x 4.6 mm, 5 μm column with the mobile phase containing ammonium carbonate and acetonitrile. The excitation and emission wavelengths were 330 and 420 nm respectively. The method was validated according to the Commission Decision 2002/657/EC and all parameters are in agreement with the requirements of the Decision. Linearity was determined for the concentration range of 25-400 μg/kg. The coefficient of determination (R2) for all curves was from 0.985 to 0.996. The limit of detection (LOD) was in the range 3.23 to 6.53 μg/kg and the limit of quantification (LOQ) from 11.78 to 13.06 μg/kg. The decision limit (CCα) ranged from 29.56 to 43.08 μg/kg and detection capability (CCβ) from 40.65 to 51.01 μg/kg. The highest coefficient of variation (CV) for repeatability was 14.3% and for reproducibility 15.4%.

scholarly journals Simultaneous determination of phytoestrogens in dietary supplements by high-performance liquid chromatography

2021 ◽  
Vol 4 (3) ◽  
pp. 24-35
Author(s):  
Thanh An Vu Thi ◽  
Thanh Hoa Mac Thi ◽  
Khanh Cao Cong ◽  
◽  
◽  
...  
Keyword(s):  
Dietary Supplements ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Ultrasonic Method ◽  
Gradient Elution ◽  
Analysis Procedure ◽  
Range Limit ◽  
Limit Of Quantification

The bio-active phytoestrogen compounds (puerarin, daidzin, glycitin, genistin, miroestrol, daidzein, glycitein, genistein) in dietary supplements were extracted by ultrasonic method with methanol solvent in 40oC. The analysis procedure was carried out on HPLC Alliance e2695 (Waters) system, with RP-C18 Reliant (25 mm × 4.6 mm; 5µm) column, at 30oC. Phytoestrogens were separated by using gradient elution with a mobile phase consisting 0.1% (v/v) phosphoric aqueous solution and methanol in 45 minutes. The method was validated by determining its specificity, linear range, limit of detection, limit of quantification, repeatability and accuracy. This method was applied succesfully to determine content of Phytoestrogens in commercial dietary supplement products.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

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