scholarly journals Development of a Rapid and Eco-Friendly UHPLC Analytical Method for the Detection of Histamine in Fish Products

2020 ◽  
Vol 17 (20) ◽  
pp. 7453
Author(s):  
Antonello Cicero ◽  
Francesco Giuseppe Galluzzo ◽  
Gaetano Cammilleri ◽  
Andrea Pulvirenti ◽  
Giuseppe Giangrosso ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Proficiency Tests ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Fish And Fishery Products ◽  
Short Time ◽  
Solid Liquid

We developed, validated, and confirmed with proficiency tests a fast ultra-high-performance liquid chromatography with diode array detector (UHPLC-DAD) method to determine histamine in fish and fishery products. The proposed method consists of two successive solid–liquid extractions: one with a dilute solution of perchloric acid (6%) and the second only with water. The instrumental analysis with UHPLC provides a very fast run time (only 6 min) with a retention time of approximately 4 min, a limit of quantification (LOQ) of 7.2 mg kg−1, a limit of detection (LOD) of 2.2 mg kg−1, a recovery around 100%, a relative standard deviation (RSD%) between 0.5 and 1.4, and an r2 of calibration curve equal to 0.9995. The method detected optimal values of the validation parameters and required a limited number of reagents in comparison to other methods reported in the literature. Furthermore, the method could detect histamine in a very short time compared with other methods. This method, in addition to being validated, precise, specific, and accurate, avoids wasting time, money, and resources, and limits the use of organic solvents.

scholarly journals ANALYTICAL METHOD BY HPLC-DAD ALLOWS QUANTIFICATION OF QUERCETIN MARKER IN STANDARDIZED EXTRACT OF ANADENANTHERA COLUBRINA VAR. CEBIL

2017 ◽  
Vol 9 (8) ◽  
pp. 47
Author(s):  
Valmir Gomes De Souza ◽  
FabrÍcio Havy Dantas De Andrade ◽  
Fabio Santos De Souza ◽  
Rui Oliveira Macedo
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Room Temperature ◽  
Limit Of Detection ◽  
Array Detector ◽  
Diode Array Detector ◽  
Limit Of Quantification ◽  
Hydroalcoholic Extract ◽  
Relative Standard ◽  
Validation Parameters

Objective: The Anadenanthera colubrina (Vell.) Brennan var. cebil is a medicinal plant that has been used for the treatment of many diseases in the northeastern region of Brazil. This plant contains secondary metabolites such as quercetin, a flavonoid that is known by its antioxidant and anti-inflammatory effects. The aim of this work is to propose the validation of an analytical method using high-performance liquid chromatography with diode array detector (HPLC-DAD) for the quantification of quercetin and standardization of the hydroalcoholic extract (HAE) of A. colubrina.Methods: The A. colubrina extracts were prepared by the maceration process with powdered leaves at 20% weight: volume (w/v) and a hydroalcoholic solution at 50% volume: volume (v/v) for 120 h at room temperature. After pretreatment of the hydroalcoholic extract, the quercetin marker was used for quantification and proceeded to the evaluation of validation parameters for the method using HPLC-DAD.Results: The analytical method proved to be specific. Linear over the range 1.4–26.6 µg/ml, regression analysis showed a good correlation coefficient (R2= 0.999); the limit of detection (LOD) and the limit of quantification (LOQ) were 0.27 and 0.81 μg/ml respectively. The relative standard deviation (RSD) did not exceed 2.5% for precision. The proposed method was validated with an average recovery of 92.5–97.5%.Conclusion: The method was validated using HPLC-DAD, allowing the quantification of quercetin in the standardisation process of extracts and quality control of the herbal drug containing A. colubrina Phyto complex.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

Nanoparticulate Mycophenolic Acid Eye Drops - Analytical Validation of a High Performance Liquid Chromatography Assay and Stability Studies

2021 ◽  
Vol 09 ◽  
Author(s):  
Ali Al-Kulabi ◽  
Louis Gooden ◽  
Ijeoma F. Uchegbu
Keyword(s):  
Mycophenolic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Immunosuppressive Agent ◽  
Plate Count ◽  
Eye Drops ◽  
Limit Of Quantification ◽  
Drug Content ◽  
Relative Standard ◽  
Validation Parameters

Background: Mycophenolic acid (MPA), an immunosuppressive agent, is used orally to reduce corneal graft rejection. However its oral use is associated with gastrointestinal side effects. Objectives: To prepare MPA nanoparticle eye drops and a validated analytical method. Methods: Aqueous MPA eye drops were prepared by nanoencapsulation of MPA using Nanomerics MET (N-palamitoylN-monomethyl-N,N-dimethyl-N,N,N-trimethyl-6-O-glycolchitosan) at a MET, MPA ratio of 7.5: 1 g g-1 in the presence of glycerol (2.75% w/w). A validated MPA in-formulation drug substance assay was then developed. Results: MET-MPA formulations were prepared as well as a validated assay. Assay validation parameters for the analysis of MPA in the formulation were satisfactory [Plate count = 16458, Capacity Factor = 2.4, Tailing Factor = 1.02, linearity = 0.999 (0.016 – 0.5 mg mL-1 ), limit of detection = 0.056 mg mL-1 , limit of quantification = 0.17 mg mL-1 , accuracy = 98%, intraday and interday relative standard deviation = 0.45% and 4% respectively]. The candidate formulation (z - average mean = 66 ± 0.4 nm, polydispersity index = 0.12 ± 0.012, drug content = 1.14 ± 0.003 mg mL-1 , zeta potential = +8.5 ± 1.4 mV, pH = 7.4 ± 0.02, osmolarity = 309 ± 1.5 mOSm L-1 , viscosity = 1.04 ± 0.001 mPa.s) was then found to be stable for 14 days with respect to drug content at refrigeration, room and accelerated (40C )temperature and. All other formulation parameters were within the ocular comfort range. Conclusions: A validated assay (ICH and US FDA guidelines) for new MPA nanoparticle eye drops has been developed.

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 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.

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.

scholarly journals Determination and validation of Tetracycline residues in Poultry by High Performance Liquid Chromatography - Diode Array Detector Technique

2019 ◽  
Vol 30 (3) ◽  
pp. 38
Author(s):  
Lobaina M Alrhia ◽  
Issam Mohamad ◽  
Sameer Mearouf
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Tetracycline Residues

The aim of this research is separation and determination of trace Tetracycline residues in Poultry chest, thigh and liver using High Performance Liquid Chromatography - Diode Array Detector (HPLC-DAD), with a mobile phase mixture consisting of acetonitrile: methanol: oxalic acid (0.01M) (25:15:60) and chromatographic column C8. The study was done on 32 live poultry individuals. All individuals were injected in the chest by 1m of Tetracycline standard solutions, then slaughter for analysis throughout four successive days. The injection with 10×103 ppb of Tetracycline showed that the traces of Tetracycline residues (according to the Codex Alimentarius Commission) exceeded the value of the maximum residue limit (MRL = 200 ppb) in the thigh and chest meat at the 1st day and the 1st & 2nd days of slay respectively, and exceeded the value of (MRL = 600 ppb) in the liver at the 3rd and 4th days of slay. limit of detection was LOD = 0.451 ppb, limit of quantification LOQ = 1.502 ppb, and recovery percentages of Tetracycline at a concentration of 200.0 ppb for 20 sample Rec.% = (88.966 - 91.055%), (84.623 - 87.667%), (82.198 - 83.688%) for Poultry chest, thigh and liver respectively with a percentage relative standard deviations (RSD%) of < 1 %.

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 Validation of developed method by RP-HPLC for estimation of Prasugrelin human plasma and studying the stability of the drugs in plasma

2018 ◽  
Vol 13 (1) ◽  
pp. 65-75
Author(s):  
Kumar S. Ashutosh ◽  
Debnath Manidipa ◽  
Rao J.V.L.N. Seshagiri ◽  
Sankar D. Gowri
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Potassium Dihydrogen Phosphate ◽  
Array Detector ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard ◽  
The Stability

This paper is concern with a reverse phase high performance liquid chromatography (RP-HPLC) bio-analytical method development and validation for Prasugrel in human plasma using photo diode array detector (PDA detector). The HPLC separation was carried out in an isocratic mode on an X-Terra C18 column (4.6 x 150 mm; 5 μm) with a mobile phase consisting of potassium dihydrogen phosphate [pH 3.0] and acetonitrile in the ratio of 30:70 v/v at a flow rate of 1.0 mL/min. The run time was maintained for 5 mins and the detection was monitored at 210 nm. The percentage recovery was found 99.61-100.06 in human plasma. This reveals that the method is quite accurate. The linearity was found 15-40 μg/mL in human plasma. The inter-day and intra-day precision in plasma was found within the limits. The lower limit of quantification (LLOQ) obtained by the proposed method was 0.05 μg/mL. The percentage relative standard deviation (%RSD) obtained for the drug spiked in plasma for stability studies were less than 2 %.Kathmandu University Journal of Science, Engineering and TechnologyVol. 13, No. 1, 2017, Page: 65-75

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF THYMOL AND EUGENOL BY USING RP-HPLC IN PURE AND IN EMULGEL FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 59-65
Author(s):  
Vinita C. Patole ◽  
Shilpa P. Chaudhari ◽  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Peak Areas ◽  
80 A 20 ◽  
Development And Validation

An attempt was made to develop a simple, selective, rapid and precise high-performance liquid chromatography (HPLC) method for simultaneous estimation of thymol and eugenol. Analysis was performed on a C18 column with the mobile phase consisting of solvent %A (water) and solvent %B (acetonitrile) with the following gradient: 0–1 min, 80 % A, 20 % B; 1–7 min, 40 % A and 60 % B; 7–12 min, 10 % A and 90 % B; and 12–15min, 80 % A and 20 % B at a flow rate of 0.6 mL/min. The compounds were well separated on a Thermo Scientific Hypersil BDS RP C18 column (4.6 mm × 150 mm, dp = 5 µm) and ultraviolet detection at 280 nm. The retention times of eugenol and thymol were 10.5 min and 11.6 min, respectively. Validation of the proposed method was carried out according to the guidelines of the International Council on Harmonization (ICH). The linearity of the method is good for thymol and eugenol over the concentration range of 1–50 ppm, and the r 2 values were 0.9996 for both thymol and eugenol. The calculated limit of detection (LOD) value was 0.5ppm and the limit of quantification (LOQ) value was 1ppm for both the analytes. The intra and interday relative standard deviation (RSD) of the retention time and peak areas was less than 3 %.The established method was appropriate, and the two markers were well resolved, enabling efficient quantitative analysis of thymol and eugenol.

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