scholarly journals A new liquid phase microextraction method-based reverse micelle for analysis of dexketoprofen in human plasma by HPLC-DAD

2020 ◽  
Vol 11 (1) ◽  
Author(s):  
Dönay Yuvali ◽  
Erkan Yilmaz ◽  
İbrahim Narin
Keyword(s):  
Liquid Phase ◽  
Human Plasma ◽  
Reverse Micelle ◽  
Limit Of Detection ◽  
Aqueous System ◽  
Aqueous Sample ◽  
Photodiode Array Detection ◽  
Limit Of Quantification ◽  
Liquid Phase Microextraction ◽  
Relative Standard

AbstractA new liquid phase microextraction method was developed by used reverse micelle-based coacervates as microextraction agents for the separation of dexketoprofen (DKT) from human plasma before its determination by high-performance liquid chromatography with photodiode-array detection (HPLC-DAD). The change in the concentration of dexketoprofen in the plasma of the male and female patients was successfully monitored by using this method. The proposed method involves the use of reverse micelles of decanoic acid (DA) are dispersed in tetrahydrofuran (THF) and aqueous system. After addition of the DA and THF to the aqueous sample phase, the formation of micelles of nano and molecular size was observed in an ultrasonic bath. The solution was centrifuged, and the DKT extracted into the DA phase was analyzed by HPLC-DAD. Some analytical parameters that important in the developed procedure were examined in detail. The limit of detection (LOD), the limit of quantification (LOQ), the intraday, and inter day relative standard deviation (RSD, %) of the developed method in the plasma sample were found to be 12.8 ng mL−1, 38.8 ng mL−1, 1.7 and 3.9%, respectively. Additional/recovery studies were performed in plasma samples with proposed method, and quantitative recoveries were obtained in the range of 97–100%. The developed microextraction method was applied to human plasma that taken from volunteer patients for the determination of DKT. Graphical abstract

Lactic Acid Determination in Human Plasma Using Ultrasound-Assisted Emulsification Microextraction Followed by Gas Chromatography

2016 ◽  
Vol 69 (4) ◽  
pp. 451 ◽  
Author(s):  
Parvin Shahdousti ◽  
Rezvan Shojaee ◽  
Mohammad Aghamohammadi ◽  
Behrang Harooni
Keyword(s):  
Gas Chromatography ◽  
Lactic Acid ◽  
Human Plasma ◽  
Limit Of Detection ◽  
Aqueous Sample ◽  
Extraction Solvent ◽  
Relative Standard ◽  
Ultrasound Assisted ◽  
Emulsification Microextraction

A rapid, sensitive, and accurate analytical method was developed for determination of lactic acid (LA) in human plasma to monitor lactic acidosis. This method was based on an ultrasound-assisted emulsification microextraction (USAEME) method followed by gas chromatography with flame ionization detection (GC–FID). Derivatization of LA was carried out by a low density alcoholic solvent which performs both as an extraction solvent and derivatization agent, simultaneously. In this procedure, 100 μL of binary mixtures of pentan-1-ol with toluene (70 : 30, v/v %) was slowly injected into a 10 mL acidified aqueous sample of LA placed into an ultrasonic water bath. The resulting emulsion was centrifuged and after derivatization, 2 μL of organic phase was analysed by GC–FID. The effective variables were evaluated to optimize the efficiency of USAEME. Under the optimum conditions, good linearity in the range of 0.06–7.77 mmol L–1 was obtained with a correlation coefficient (R2) of 0.991 and a limit of detection (LOD) of 0.04 mmol L–1 for water samples. The inter-day and intra-day repeatability of the proposed method in human plasma were evaluated in terms of the relative standard deviation (RSD %) and were found to be <10 %. The results revealed that the USAEME–GC–FID method can be applied successfully for determination of LA in human plasma samples with satisfactory accuracy and precision.

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%).

Development and Validation of a New Method for the Determination of Anti-hepatitis C Agent Simeprevir in Human Plasma using HPLC with Fluorescence Detection

2020 ◽  
Vol 16 (4) ◽  
pp. 428-435
Author(s):  
Ahmed F.A. Youssef ◽  
Yousry M. Issa ◽  
Kareem M. Nabil
Keyword(s):  
Hepatitis C ◽  
Human Plasma ◽  
Fluorescence Detection ◽  
Internal Standard ◽  
Protein Precipitation ◽  
Assay Method ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Relative Standard

Background: Simeprevir is one of the recently discovered drugs for treating hepatitis C which is one of the major diseases across the globe. Objective: The present study involves the development of a new and unique High-Performance Liquid Chromatography (HPLC) method using fluorescence detection for the determination of simeprevir (SIM) in human plasma. Methods: Two methods of extractions were tested, protein precipitation using acetonitrile and liquidliquid extraction. A 25 mM dipotassium hydrogen orthophosphate (pH 7.0)/ACN (50/50; v/v), was used as mobile phase and C18 reversed phase column as the stationary phase. The chromatographic conditions were optimized and the concentration of simeprevir was determined by using the fluorescence detector. Cyclobenzaprine was used as an internal standard. Results: Recovery of the assay method based on protein precipitation was up to 100%. Intra-day and inter-day accuracies range from 92.30 to 107.80%, with Relative Standard Deviation (RSD) range 1.65-8.02%. The present method was successfully applied to a pharmacokinetic study where SIM was administered as a single dose of 150 mg SIM/capsule (Olysio®) to healthy individuals. Conclusion: This method exhibits high sensitivity with a low limit of quantification 10 ng mL-1, good selectivity using fluorescence detection, wide linear application range 10-3000 ng mL-1, good recovery and highly precise and validation results. The developed method can be applied in routine analysis for real samples.

scholarly journals Stability-indicating HPLC-DAD assay for simultaneous quantification of hydrocortisone 21 acetate, dexamethasone, and fluocinolone acetonide in cosmetics

2020 ◽  
Vol 18 (1) ◽  
pp. 962-973
Author(s):  
Saira Arif ◽  
Sadia Ata
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Fluocinolone Acetonide ◽  
Internal Diameter ◽  
Forced Degradation ◽  
Specific Method ◽  
Regression Equations ◽  
Limit Of Quantification ◽  
Simultaneous Quantification ◽  
Relative Standard

AbstractA rapid and specific method was developed for simultaneous quantification of hydrocortisone 21 acetate (HCA), dexamethasone (DEX), and fluocinolone acetonide (FCA) in whitening cream formulations using reversed-phase high-performance liquid chromatography. The effect of the composition of the mobile phase, analysis temperature, and detection wavelength was investigated to optimize the separation of studied components. The analytes were finally well separated using ACE Excel 2, C18 AR column having 150 mm length, 3 mm internal diameter, and 2 µm particle size at 35°C using methanol with 1% formic acid and double-distilled deionized water in the ratio of 60:40 (v/v), respectively, as the mobile phase in isocratic mode. Ten microliters of sample were injected with a flow rate of 0.5 mL/min. The specificity, linearity, accuracy, precision, recovery, limit of detection (LOD), limit of quantification (LOQ), and robustness were determined to validate the method as per International Conference on Harmonization guidelines. All the analytes were simultaneously separated within 8 min, and observed retention times of HCA, DEX, and FCA were 4.5, 5.5, and 6.9 min, respectively. The proposed method showed good linearity with the correlation coefficient, R2 = 0.999 over the range of 1–150 µg/mL for all standards. The linear regression equations were y = 12.7x + 118.7 (r = 0.999) for HCA, y = 12.9x + 106.8 (r = 0.999) for DEX, and y = 12.9x + 96.8 (r = 0.999) for FCA. The LOD was 0.25, 0.20, and 0.08 µg/mL for HCA, FCA, and DEX and LOQ was 2.06, 1.83, and 1.55 µg/mL for HCA, FCA, and DEX, respectively. The recovery values of HCA, DEX, and FCA ranged from 100.7–101.3, 102.0–102.6, and 100.2–102.0%, respectively, and the relative standard deviation for precision (intra- and interday) was less than 2, which indicated repeatability and reproducibility. The novelty of the method was described by forced degradation experimentation of all analytes in the combined form under acidic, basic, oxidative, and thermal stress. The proposed method was found to be simple, rapid, and reliable for the simultaneous determination of HCA, DEX, and FCA in cosmetics.

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 A highly sensitive octopus-like azobenzene fluorescent probe for determination of abamectin B1 in apples

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Zhenlong Guo ◽  
YiFei Su ◽  
Kexin Li ◽  
MengYi Tang ◽  
Qiang Li ◽  
...  
Keyword(s):  
Fluorescent Probe ◽  
Limit Of Detection ◽  
Quantitative Detection ◽  
Fluorescence Signal ◽  
Ionization Mass ◽  
Limit Of Quantification ◽  
Visible Absorption ◽  
Esi Ms ◽  
Relative Standard ◽  
Ft Ir

AbstractThe development of detecting residual level of abamectin B1 in apples is of great importance to public health. Herein, we synthesized a octopus-like azobenzene fluorescent probe 1,3,5-tris (5′-[(E)-(p-phenoxyazo) diazenyl)] benzene-1,3-dicarboxylic acid) benzene (TPB) for preliminary detection of abamectin B1 in apples. The TPB molecule has been characterized by ultraviolet–visible absorption spectrometry, 1H-nuclear magnetic resonance, fourier-transform infrared (FT-IR), electrospray ionization mass spectroscopy (ESI-MS) and fluorescent spectra. A proper determination condition was optimized, with limit of detection and limit of quantification of 1.3 µg L−1 and 4.4 μg L−1, respectively. The mechanism of this probe to identify abamectin B1 was illustrated in terms of undergoing aromatic nucleophilic substitution, by comparing fluorescence changes, FT-IR and ESI-MS. Furthermore, a facile quantitative detection of the residual abamectin B1 in apples was achieved. Good reproducibility was present based on relative standard deviation of 2.2%. Six carboxyl recognition sites, three azo groups and unique fluorescence signal towards abamectin B1 of this fluorescent probe demonstrated reasonable sensitivity, specificity and selectivity. The results indicate that the octopus-like azobenzene fluorescent probe can be expected to be reliable for evaluating abamectin B1 in agricultural foods.

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.

ESTIMATION OF TADALAFIL IN HUMAN PLASMA BY SPECTROFLUOROPHOTOMETRY

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (06) ◽  
pp. 60-63
Author(s):  
Sadhana Rajput ◽  
◽  
Samir Patel ◽  
Keyword(s):  
Human Plasma ◽  
Fluorescence Spectrum ◽  
Drug Monitoring ◽  
Limit Of Detection ◽  
Wave Length ◽  
Excitation Wavelength ◽  
Limit Of Quantification ◽  
Pharmacokinetic Investigation ◽  
Satisfactory Recovery

A new, specific, selective, simple, rapid and inexpensive spectrofluorophotometric method has been developed for the determination of tadalafil in spiked human plasma. The fluorescence spectrum of tadalafil in 0.1M methanolic sulphuric acid showed excitation wavelength at 315 nm and emission wave-length at 332 nm. The method for tadalafil was found to be linear over the concentration range of 10-50 ng/mL with a correlation coefficient of 0.9991. Limit of detection and limit of quantification were found to be 0.235 ng/mL and 0.701 ng/mL, respectively. The method was validated and found to be suitable for the estimation of tadalafil from human plasma. Satisfactory recovery of tadalafil from the human plasma suggests no interference of any debris present into human plasma. This method can be used to deter-mine plasma tadalafil concentration in drug monitoring or pharmacokinetic investigation.

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