Simultaneous Quantitation of Five Bioactive Ingredients in Raw and Processed Fallopia multiflora by Employing UHPLC-Q-TOF-MS

2019 ◽  
Vol 57 (7) ◽  
pp. 618-624
Author(s):  
Yi Tao ◽  
Xiaoping Zhou ◽  
Weidong Li ◽  
Baochang Cai
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Bioactive Components ◽  
Limit Of Quantification ◽  
Sample Handling ◽  
Flight Mass Spectrometry ◽  
Relative Standard ◽  
Bioactive Ingredients ◽  
Aqueous Formic Acid

Abstract Fallopia multiflora is used for treatment of premature graying hair and blood deficiency. In this study, a quantitative method was developed for determination of five bioactive components (emodin, 2,3,5,4′-tetrahydroxy-stilbene- 2-Ο-β-d-glucoside, emodin-8-O-β-d-glucopyranoside, ω-hydroxyemodin and kaempferol) in raw and processed F. multiflora by using ultra-high performance liquid chromatography (UHPLC)-quadrupole time-of-flight mass spectrometry-based method. The sample handling procedure was optimized. Chromatographic separation was carried out on a Thermo Syncronis AQ-C18 UHPLC column with mobile phase consisting of 0.01% aqueous formic acid and acetonitrile. The method was interrogated in terms of linearity, precision, stability and recovery tests. All calibration curves displayed good linearity (R2 > 0.9992). The limit of detection and limit of quantification of these components ranged from 0.01 to 0.03 μg/mL and from 0.03 to 0.07 μg/mL, respectively. The average recoveries of these components were from 98.2 to 102.9% with relative standard deviation values from 0.8 to 2.9% for F. multiflora. The developed method can be applied to quality control of raw and processed F. multiflora.

scholarly journals Micelle-Mediated Extraction Prior to LC-UV for Preconcentration and Determination of Trace Amounts of Bisphenol A in Environmental Samples

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Naghi Saadatjou ◽  
Shahab Shariati ◽  
Mostafa Golshekan
Keyword(s):  
Bisphenol A ◽  
High Performance ◽  
Limit Of Detection ◽  
Aqueous Samples ◽  
Limit Of Quantification ◽  
Rich Phase ◽  
Factors Affecting ◽  
Relative Standard ◽  
Triton X

A simple and high sensitive preconcentration method based on micelle-mediated extraction followed by high performance liquid chromatography (LC-UV) was developed for preconcentration and determination of trace amounts of bisphenol A (BPA) in aqueous samples. The BPA was quantitatively extracted from aqueous samples in the presence of Triton X-114 as a nonionic surfactant and preconcentrated into the small volume (about 30 μL) of the surfactant-rich phase. Taguchi method, an orthogonal array design (OA16 (45)), was utilized to optimize the various factors affecting the micellar extraction of BPA. The maximum extraction efficiency of BPA was obtained at pH 3, 0.2% (w/v) Triton X-114, and 0.25 mol L−1 sodium acetate. For the preconcentration, the solutions were incubated in a thermostatic water bath at 50°C for 7 min. After centrifuge and separation of aqueous phase, the surfactant-rich phase was diluted with 100 μL acetone and injected in the chromatographic system. Under the optimum conditions, preconcentration factor of 34.9 was achieved for extraction from 10 mL of sample solution and the relative standard deviation (RSD%) of the method was lower than 6.6%. The calibration curve was linear in the range of 0.5–150 μg L−1 with reasonable linearity (r2>0.9987). The limit of detection (LOD) based on S/N = 3 was 0.13 μg L−1 for 10 mL sample volumes. The limit of quantification (LOQ) based on S/N = 10 was 0.43 μg L−1 for 10 mL sample volumes. Finally, the applicability of the proposed method was evaluated by the extraction and determination of BPA in the real samples, and satisfactory results were obtained.

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 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.

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 Development of a QuEChERS-Based UHPLC-MS/MS Method for Simultaneous Determination of Six Alternaria Toxins in Grapes

Toxins ◽  
2019 ◽  
Vol 11 (2) ◽  
pp. 87 ◽  
Author(s):  
Wenbo Guo ◽  
Kai Fan ◽  
Dongxia Nie ◽  
Jiajia Meng ◽  
Qingwen Huang ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Safe Procedure ◽  
Alternariol Monomethyl Ether ◽  
Limit Of Quantification ◽  
Alternaria Toxins ◽  
Relative Standard

A simple and reliable analytical method for the simultaneous determination of alternariol (AOH), altenuene (ALT), tentoxin (TEN), altenusin (ALS), tenuazonic acid (TeA), and alternariol monomethyl ether (AME) in grapes was developed by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure with the extraction by acetonitrile and purification by sodium chloride (0.5 g) and anhydrous magnesium sulfate (0.5 g) was established to recover the six Alternaria toxins. After validation by determining the linearity (R2 > 0.99), recovery (77.8–101.6%), sensitivity (limit of detection in the range of 0.03–0.21 μg kg−1, and limit of quantification in the range of 0.09–0.48 μg kg−1), and precision (relative standard deviation (RSD) ≤ 12.9%), the analytical method was successfully applied to reveal the contamination state of Alternaria toxins in grapes. Among 56 grape samples, 40 (incidence of 71.4%) were contaminated with Alternaria toxins. TEN was the most frequently found mycotoxin (37.5%), with a concentration range of 0.10–1.64 μg kg−1, followed by TeA (28.6%) and AOH (26.8%). ALT (10.7%), AME (3.6%), and ALS (5.4%) were also detected in some samples. To the best of our knowledge, this is the first report about the Alternaria toxins contamination in grapes in China.

scholarly journals Vortex Assisted Liquid-Liquid Microextraction with Back Extraction of Repaglinide, Glibenclamide and Glimepiride in Water Samples

2021 ◽  
Vol 50 (5) ◽  
pp. 1297-1307
Author(s):  
Sohaib Jumaah Owaid Luhaib ◽  
Noorfatimah Yahaya ◽  
Anas Alshishani ◽  
Maizatul Najwa Jajuli ◽  
Mazidatulakmam Miskam
Keyword(s):  
Water Samples ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Aqueous Sample ◽  
Back Extraction ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Liquid Microextraction

A new analytical method based on vortex-assisted liquid-liquid microextraction with back extraction (VALLME-BE) coupled with high performance liquid chromatography was developed for the simultaneous determination of antidiabetic drugs; repaglinide, glibenclamide, and glimepiride in water samples. Chromatographic separation was achieved using C18 column (250 × 4.6 mm × 5 µm) and methanol-phosphate buffer (pH3.7) in the ratio of 70:30 v/v as a mobile phase at a flow rate of 1 mLmin-1. VALLME-BE was performed using 200 μL of n-octane dispersed into the aqueous sample (10 mL) with the aid of vortexing agitation. Then, the analytes were back-extracted from the organic solvent to 0.05 M NaOH (40 µL). Under these conditions, enrichment factor of 155-fold was achieved. The developed VALLME-BE method showed excellent linearity in the range of 30 to 1000 µgL-1 with limit of detection (LOD) of 0.41-1.66 µgL-1 and limit of quantification (LOQ) of 1.38-5.54. 41-1.66 µgL-1. VALLME-BE was applied for the determination of repaglinide, glibenclamide and glimepiride in water samples with the recoveries ranged from 83-109%. The relative standard deviation for inter-day and intra-day precision was less than 9.9%.

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 A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

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>

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

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