Preconcentration and determination of ranitidine hydrochloride in real samples by using modified magnetic iron oxide nanoparticles

2016 ◽  
Vol 94 (1) ◽  
pp. 9-14 ◽  
Author(s):  
Elaheh Konoz ◽  
Amir H.M. Sarrafi ◽  
Hamed Sahebi
Keyword(s):  
Human Plasma ◽  
Ph Value ◽  
Limit Of Detection ◽  
Solid Phase ◽  
High Surface ◽  
Sodium Dodecyl ◽  
Magnetic Iron Oxide Nanoparticles ◽  
Ranitidine Hydrochloride ◽  
Relative Standard

This method shows a novel, fast, and simple magnetic solid-phase extraction (SPE) and spectrophotometric procedure for preconcentration and determination of ranitidine hydrochloride in human plasma and aquatic samples by using Fe3O4 nanoparticles (NPs) modified by sodium dodecyl sulfate (SDS) as an extractor. The unique properties of Fe3O4 NPs including high surface area and strong magnetism were utilized effectively in the magnetic SPE process. The determination method is based on the SDS-coated Fe3O4 NPs with extracted ranitidine-HCl, which was subsequently monitored spectrophotometrically at λmax = 320 nm. Effects of different parameters influencing the extraction efficiency of ranitidine-HCl including the pH value, amount of SDS, and Fe3O4 NPs, extraction time, desorption solvent, desorption time, and sample volume were optimized. Under optimized conditions, the method was successfully applied to the extraction of ranitidine-HCl from human plasma and aquatic samples. The extraction recovery in human plasma and different matrixes of waters were investigated and values of 89.0%–103.4% were obtained. The calibration graph for the determination of ranitidine-HCl was linear in the range of 0.025–1.50 μg mL−1 with R2 = 0.9946. The limit of detection of the proposed method was 7.5 × 10−3 μg mL−1. The repeatability and reproducibility (relative standard deviation) of the mentioned method were 0.83% and 1.22%, respectively. The experimental results showed that the proposed method was feasible for the analysis of ranitidine-HCl in environmental and biological samples.

Micellar-Enhanced Spectrofluorimetric Method for Quantification of Diclofenac Potassium in Pure Form, in Pharmaceutical Preparations and Human Plasma

2021 ◽  
Vol 58 (6) ◽  
pp. 427-434
Author(s):  
Muhammad Naeem Khan ◽  
Irum ◽  
Saba Gul ◽  
Muslima ◽  
Muhammad Mursaleen
Keyword(s):  
Human Plasma ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Products ◽  
Pure Form ◽  
Fluorescence Signal ◽  
Spectrofluorimetric Method ◽  
Relative Standard

Abstract A rapid, simple and economical spectrofluorimetric method for the determination of diclofenac potassium in pure form, in pharmaceutical preparations and in human plasma has been developed. The method is based on the enhancement of the fluorescence signal of diclofenac potassium by the addition of sodium dodecyl sulphate in McIvaine buffer with a pH of 5. Different experimental conditions such as buffer type, pH, type and concentration of surfactants were investigated. The fluorescence intensity of the solution was recorded at 361 nm after excitation at 243 nm. The method shows linearity in the concentration range of 0.2 μg mL–1–10 μg mL–1 with a good correlation coefficient of 0.997. The relative standard deviation value was 3.62 (n = 7). The limit of detection and limit of quantification were calculated to be 2.84 × 10–3 μg mL–1 and 9.47 × 10–3 μg mL-1, respectively. The effect of excipients and co-administrated drugs was investigated and no interference was observed. The method was successfully applied for the determination of diclofenac potassium in pure form, in pharmaceutical products and in human plasma. The percentage recoveries obtained ranged from 100.25% to 102.16% for pure form and 97.50% to 102.00% for pharmaceutical products and from 98.50% to 101.67% for human plasma.

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.

scholarly journals Analysis of the Chloroacetanilide Herbicides in Water Using SPME with CAR/PDMS and GC/ECD

2005 ◽  
Vol 88 (4) ◽  
pp. 1236-1241 ◽  
Author(s):  
Ying-Ming Hwang ◽  
Yih-Gang Wong ◽  
Wu-Hsiung Ho
Keyword(s):  
Humic Acid ◽  
Ph Value ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Standard Addition ◽  
Electron Capture Detection ◽  
Detection Analysis ◽  
Salt Addition ◽  
Chloroacetanilide Herbicides ◽  
Relative Standard

Abstract The solid-phase microextraction (SPME) technique using a 75 mm film of carboxen/polydimethylsiloxane was applied to the analysis of chloroacetanilide herbicides (acetochlor, alachlor, butachlor, metolachlor, and propachlor) residues. The feasibility of SPME with gas chromatography electron capture detection analysis has been evaluated. The effects of experimental parameters such as magnetic stirring, salt addition, humic acid addition, pH value, and extraction time, as well as desorption temperature and time, were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The inhibition of humic acid to the extraction of chloroacetanilide herbicides was observed. A standard addition method for calibration was recommended to reduce deviations caused by matrix interferences. The proposed method provided a simple and rapid analytical procedure for chloroacetanilide herbicides in water with limits of detection 0.002–0.065 μg/L for deionized water, and 0.005–0.22 μg/L for farm water. The relative standard deviations (n = 5) for analyses of farm water were 7–20% for 0.5 μg/L chloroacetanilide herbicides. This application was illustrated by the analysis of sample collected from farm water in the Chung-hwa area, Taiwan.

scholarly journals Spectrophotometric Determination of Iron(II) after Solid Phase Extraction of Its 2,2′ Bipyridine Complex on Silica Gel-Polyethylene Glycol

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Nahid Pourreza ◽  
Saadat Rastegarzadeh ◽  
Ali Reza Kiasat ◽  
Hossein Yahyavi
Keyword(s):  
Polyethylene Glycol ◽  
Solid Phase Extraction ◽  
Silica Gel ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Calibration Graph ◽  
Phase Extraction ◽  
Relative Standard

A new solid phase extraction procedure was developed for preconcentration of iron(II) using silica gel-polyethylene glycol (silica-PEG) as an adsorbent. The method is based on retention of iron(II) as 2,2′ bipyridine complex on silica-PEG. The retained complex is eluted by 1.0 mol L−1of sulfuric acid-acetone mixture (1:2) and its absorbance is measured at 518 nm, spectrophotometrically. The effects of different parameters such as pH, concentration of the reagent, eluting reagent, sample volume, amount of adsorbent, and interfering ions were investigated. The calibration graph was linear in the range of 1–60 ng mL−1of iron(II). The limit of detection based on3Sbwas 0.57 ng mL−1and relative standard deviations (R.S.D) for ten replicate measurements of 12 and 42 ng mL−1of iron(II) were 2.4 and 1.7%, respectively. The method was applied to the determination of of iron(II) in water, multivitamin tablet, and spinach samples.

scholarly journals Application of Packed-nanofibers Solid-phase Extraction for Determination of Rhodamine B in Sausage

2019 ◽  
Vol 8 (1) ◽  
pp. 17-21
Author(s):  
Lanlan Wei ◽  
Jianjun Deng ◽  
Tao Kang ◽  
Xuejun Kang
Keyword(s):  
Rhodamine B ◽  
High Performance ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Volume Ratio ◽  
Standard Curve ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for the determination of Rhodamine B in sausage was developed and validated. After extraction of Rhodamine B with acetonitrile from foodstuffs, a novel electrospun polymer nanofibers packed micro-column was used for cleaning and concentrating of the analyte in the sample. High performance liquid chromatography with fluorescence detection (HPLC-Flu) was used for the determination of Rhodamine B in the sample. The mobile phase was composed of 3.0 g L-1 phosphate buffer and methanol (3:7, volume ratio), and the pH was adjusted to 7. 0 with orthophosphoric acid. The results showed that the standard curve was linear over the validated concentrations range of 2-500 ng g-1, and the limit of detection (LOD) and the limit of quantitation (LOQ) for Rhodamine B spiked samples was 0. 2 ng g-1 and 0. 7 ng g-1, respectively. The average recoveries of Rhodamine B were 90.4% -94.3% for sausage, and the relative standard deviation of the method was from 1.7% to 3.8%. This proposed method was applied to real sample, and there was no Rhodamine B found in sausage.

scholarly journals Microextraction by Packed Molecularly Imprinted Polymer Combined Ultra-High-Performance Liquid Chromatography for the Determination of Levofloxacin in Human Plasma

2019 ◽  
Vol 2019 ◽  
pp. 1-9 ◽  
Author(s):  
Jia Meng ◽  
Xu Wang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Bacterial Infections ◽  
High Performance ◽  
Limit Of Detection ◽  
Binding Capacity ◽  
Molecularly Imprinted ◽  
Relative Standard

Fluoroquinolones are considered as gold standard for the prevention of bacterial infections. To improve assessment of antibacterial efficacy, a novel method for determination of levofloxacin was developed and validated. Deep eutectic solvents (DESs) as only green solvent were used as a porogen for preparation of water-compatible molecularly imprinted polymers (MIPs) with a pseudotemplate. The DESs-MIPs were characterized in detail, including scanning electron microscope, nitrogen sorption porosimetry, and Fourier transform-infrared spectra. Clearly, the maximum binding capacity of levofloxacin on DESs-MIPs in water and methanol was 0.216 and 0.077 μmol g−1, respectively. The DESs-MIPs as adsorbing materials were applied in microextraction by packed sorbent (MEPS), and the DESs-MIPs-MEPS conditions were optimized. The DESs-MIPs-MEPS coupled with ultra-high-performance liquid chromatography (UHPLC) was used to determine levofloxacin in human plasma. The method was found linear over 0.05–10 μg mL−1 with coefficient of correlation equal to 0.9988. The limit of detection and limit of quantification were 0.012 and 0.04 μg mL−1, respectively. At three spiked levels, the precision of proposed method was between 95.3% and 99.7% with intraday and interday relative standard deviations ≤8.9%. Finally, the developed method was used to examine levofloxacin from human plasma of 20 hospitalized patients after transrectal ultrasound-guided prostate biopsy, and the average concentration (±SD) of levofloxacin was 2.35 ± 0.99 μg mL−1 in plasma.

Vortex-Assisted Dispersive Liquid–Liquid Microextraction Coupled with Deproteinization for Determination of Nateglinide in Human Plasma Using HPLC/UV

2020 ◽  
Author(s):  
Mohamed A Hammad ◽  
Amira H Kamal ◽  
Reham E Kannouma ◽  
Fotouh R Mansour
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
Signal To Noise Ratio ◽  
Cost Effective ◽  
Salt Addition ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

Abstract A validated method for preconcentration and determination of nateglinide in plasma was developed using vortex-assisted dispersive liquid–liquid microextraction. Different variables that affect extraction efficiency were studied and optimized, including type and volume of extractant, type and volume of disperser, pH of diluent, salt addition effect, centrifugation and vortex time. Nateglinide was extracted using 30 μL of 1-octanol as an extractant and 200 μL of methanol as a disperser. The enrichment factor reached 330 under the optimum conditions. High-performance liquid chromatography/ultraviolet was used for detection using phosphate buffer (pH 2.5, 10 mM): acetonitrile (45:55, v/v) as a mobile phase at a flow rate of 1 mL/min. The method was linear over the range of 50–20,000 ng/mL with a limit of detection of 15 ng/mL (signal-to-noise ratio = 3). Intra- and inter-day precision had %relative standard deviation <6% (n = 3) and the %recoveries were found to be between 102.5 and 105.9%. The proposed method is simple, sensitive, eco-friendly, cost-effective and powerful for microextraction of nateglinide from human plasma samples.

Simultaneous Determination of Cationic and Anionic Surfactants in Domestic, Sewage and River Effluent by Diffuse Reflectance -Fourier Transform Infrared Spectroscop ic Analysis

2021 ◽  
Vol 30 (1) ◽  
pp. 32-40 ◽  
Author(s):  
Ramsingh Kurrey ◽  
Kaushlya Thakur ◽  
Swati Chandrawanshi ◽  
Manas Kanti Deb
Keyword(s):  
Fourier Transform ◽  
Standard Deviation ◽  
Simultaneous Determination ◽  
Diffuse Reflectance ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Fourier Transform Infrared ◽  
Domestic Sewage ◽  
Relative Standard

A new, simple, rapid and precise novel hyphenated diffuse reflectance-Fourier transform infrared spectroscopy (DRS-FTIR) technique for the simultaneous determination of the most frequently used cationic surfactants (CS+) i.e. cetyltrimethylammonium bromide (CTAB) and anionic surfactant (AS-) i.e. sodium dodecyl sulphate (SDS) in domestic, sewage and river wastewater samples has been stabilised. CS+ and AS- were analyzed using DRS-FTIR, the most steady and strongest vibrational IR peak at 2917.13 cm-1 for CTAB and 1226.07 for SDS were selected for the simultaneous quantiflcation of CS+ and AS- under the optimized condition such as effect of samples volume and effect of temperature. The limit of detection (LOD) and limit of quantiflcation (LOQ) of the present method were 5 µg/mL and 15 µg/mL, respectively. The absorbance and peak area were determined by the DRS-FTIR method, which shows excellent linearity with a correlation coefflcient value of 0.985 and 0.981 for the concentration range of 10-100 µg/mL. The standard deviation (SD) and relative standard deviation (RSD) for six replicate measurements were found to be 0.052 µg/L and 2.8 %, respectively.

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 Determination of Ivermectin in Salmon Muscle Tissue by Liquid Chromatography with Fluorescence Detection

1998 ◽  
Vol 81 (3) ◽  
pp. 549-553 ◽  
Author(s):  
Heidi S Rupp ◽  
Sherri B Turnipseed ◽  
Calvin C Walker ◽  
José E Roybal ◽  
Austin R Long
Keyword(s):  
Atlantic Salmon ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Average Concentration ◽  
Baseline Noise ◽  
Muscle Tissues ◽  
Relative Standard ◽  
Fluorescent Moiety ◽  
Liquid Chromatographic

abstract A liquid chromatographic method was developed for determination of ivermectin B1a (IVR) extracted from raw fortified and incurred Atlantic salmon muscle tissues. The method was also used to determine fortified doramectin (DOR) in Atlantic salmon. Tissue extract was applied to a C8 solid-phase extraction (SPE) column, followed by a silica SPE column. Residues in the eluate were treated with trifluoroacetic anhydride and methylimidazole to dehydrate the IVR molecule and form an aromatic fluorescent moiety with a trifluoroacetic ester. This product was subsequently treated with ammonium acetate in methanol to cleave the ester and convert the functional group back to a stable alcohol form. The analytes were determined by fluorescence with excitation at 272 nm and emission at 465 nm. A Cis Hypersil column was used for analysis with a mobile phase of acetonitrile-water (90 + 10, v/v) and an oven temperature of 65°C. IVR and DOR were determined at 5 fortification levels (1, 5,10, 20, and 40 ppb). Intra-assay absolute recoveries ranged from 75 to 89% for IVR and from 73 to 85% for DOR. Relative standard deviations (RSDs) were &lt;7% in all cases. The limit of detection (3 x baseline noise) was 0.25 ppb extracted from tissue. Incurred tissues had an average concentration of 32 ppb, with an RSD of 3%.

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