scholarly journals Determination of Residual Nonsteroidal Anti-Inflammatory Drugs in Aqueous Sample Using Magnetic Nanoparticles Modified with Cetyltrimethylammonium Bromide by High Performance Liquid Chromatography

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Malihe Khoeini Sharifabadi ◽  
Mohammad Saber-Tehrani ◽  
Syed Waqif Husain ◽  
Ali Mehdinia ◽  
Parviz Aberoomand-Azar

A simple and sensitive solid-phase extraction method for separation and preconcentration of trace amount of four nonsteroidal anti-inflammatory drugs (naproxen, indomethacin, diclofenac, and ibuprofen) using Fe3O4magnetic nanoparticles modified with cetyltrimethylammonium bromide has been developed. For this purpose, the surface ofMNPswas modified with cetyltrimethylammonium bromide (CTAB) as a cationic surfactant. Effects of different parameters influencing the extraction efficiency of drugs including the pH, amount of salt, shaking time, eluent type, the volume of solvent, amount of adsorbent, sample volume, and the time of desorption were investigated and optimized. Methanol has been used as desorption solvent and the extracts were analysed on a reversed-phase octadecyl silica column using 0.02 M phosphate-buffer (pH = 6.02) acetonitrile (65 : 35 v/v) as the mobile phase and the effluents were measured at 202 nm with ultraviolet detector. The relative standard deviation (RSD%) of the method was investigated at three concentrations (25, 50, and 200 ng/mL) and was in the range of 3.98–9.83%(n=6)for 50 ng/mL. The calibration curves obtained for studied drugs show reasonable linearity(R2>0.99)and the limit of detection(LODs)ranged between 2 and 7 ng/mL. Finally, the proposed method has been effectively employed in extraction and determination of the drugs in biological and environmental samples.

2018 ◽  
Vol 5 (7) ◽  
pp. 171311 ◽  
Author(s):  
Syed Fariq Fathullah Syed Yaacob ◽  
Muhammad Afzal Kamboh ◽  
Wan Aini Wan Ibrahim ◽  
Sharifah Mohamad

A magnetic solid-phase extraction (MSPE) procedure on the newly synthesized magnetic β-cyclodextrin functionalized with toluene diisocyanate (TDI) as a linker and further modified with bio-polymeric spores of sporopollenin (MSp-TDI-βCD), was developed for the extraction of nonsteroidal anti-inflammatory drugs (NSAIDs), namely, indoprofen (INP), ketoprofen (KTP), ibuprofen (IBP) and fenoprofen (FNP) from water samples prior to their HPLC-DAD determination. The newly synthesized MSp-TDI-βCD was comprehensibly characterized using FT-IR, XRD, SEM-EDX, BET and VSM analyses. The separation of selected NSAIDs on MSp-TDI-βCD from aqueous solution was simply achieved by applying an external magnetic field via a permanent magnet. The MSPE parameters affecting extraction performance, i.e. sorbent dosage, sample volume, extraction and desorption time, type of organic eluent and volume and solution pH were investigated and optimized. The proposed method showed linear range between 0.5 and 500 ng ml −1 , low limit of detection at S/N = 3 (0.16–0.37 ng ml −1 ) and limit of quantification at S/N = 10 (0.53–1.22 ng ml −1 ). The inter-day ( n =  15) and intra-day ( n =  5) precision for the proposed methods given by relative standard deviation (RSD%) was in the range of 2.5–4.0 and 2.1–5.5, respectively. The extraction recoveries of NSAIDs from environmental samples (tap, drinking and river water) ranged from 92.5% to 123.6%, with satisfactory precision (RSD% less than 12.4%).


Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  

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.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Nahid Pourreza ◽  
Saadat Rastegarzadeh ◽  
Ali Reza Kiasat ◽  
Hossein Yahyavi

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.


2013 ◽  
Vol 800 ◽  
pp. 166-172
Author(s):  
Xiong Zhi Wu ◽  
Li Li ◽  
Fei Ping Li ◽  
Wen Ying Jin

A new sorbent (PAMAM4.0GASG) with gallic acid as functional group has been prepared based on G4.0 polyamidoamine dendrimer modified silica gel (PAMAM4.0SG) and characterized with FTIR. It was employed for selective separation, preconcentration and determination of lead in different samples by flame atomic absorption spectrometry (FAAS). Experimental conditions for effective separation and preconcentration of lead were optimized. The preconcentration factor reaches 200 for lead. The relative standard deviation (R.S.D.) under optimum conditions was 2.1% for 5.0 μg ml1 of Pb (II).The relative standard deviation (R.S.D.) was 2.1% for 5.0 μg ml1 of Pb (II). The limit of detection (LOD) of 0.081μg ml1 was achieved with a sample loading flow rate of 4.2 ml min1 and a 10 ml sample volume in the proposed method. The proposed column enrichment method was applied for the preconcentration/separation and determination of Pb (II) in tap water and river water samples successfully.


2019 ◽  
Vol 8 (1) ◽  
pp. 17-21
Author(s):  
Lanlan Wei ◽  
Jianjun Deng ◽  
Tao Kang ◽  
Xuejun Kang

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.


2020 ◽  
Vol 103 (6) ◽  
pp. 1478-1485
Author(s):  
Abdullah Taner Bişgin

Abstract Background Brilliant blue (BB) and tartrazine (TZ) are manufactured from petroleum and its products. These are the most popular consumed food dyes and are widely used in foodstuffs. Therefore, overuse of these dyes in foodstuffs and consumption of excessive amounts of these dyes can lead to health problems in humans. Objective The aim of this study was to develop a simple separation and preconcentration method for simultaneous spectrophotometric determination of BB and TZ dyes. Methods A column solid-phase separation extraction method combined with UV-Vis spectrophotometry was preferred and developed for single and simultaneous determination of BB and TZ dyes. Results The preconcentration factor was obtained as 80. Relative standard deviations were below than 4%. Detection limits of the method were determined as 0.29 and 1.21 µg/L for BB and TZ, respectively. Recovery values were obtained between 95–99% and 96–100% for BB and TZ, respectively. 10.9–235.7 µg/g and 1.7–8.0 µg/mL of BB contents of real samples were determined for solid and liquid samples, respectively. TZ concentrations of solid and liquid samples were ranged between 18.7–220.7 µg/g and 5.9–7.5 µg/mL, respectively. Conclusions Quantitative extraction results and satisfactory recovery values showed that method was successful and applicable for determination of BB and TZ concentrations in real pharmaceutical, industrial, and foodstuff samples. Highlights The method has exhibited a high preconcentration factor and effective separation against to matrix ions. The method did not need an experienced operator with high operation experience. Elution solvent can be chosen according to the availability of the chemicals in the laboratory and cheapness of the chemicals.


2013 ◽  
Vol 15 (4) ◽  
pp. 431-439 ◽  

<p>In this study, surface and wastewater in Çorlu, Tekirdağ has been monitored for ibuprofen, naproxen and diclofenac as non-steroidal anti-inflammatory drugs (NSAIDs), salicylic acid as an analgesic and caffeine. For this goal, samples were collected from 5 areas during winter and summer times (W1, W2, W3, W4 and W5) working in the field of a wastewater treatment plant site, only Çerkezköy industrial district W4. Different solid-phase extractions, pH and derivatization conditions were tested with some anti-inflammatory drugs and caffeine of Gas-Chromatography-Mass Spectrometry in environment samples and their identification and quantification at trace levels were made (ng L-1). Diclofenac (LOQ = 4.3 ng L-1) and ibuprofen (LOQ = 134.1 ng L-1) could not be determined. Other concentration levels of arranged drugs range between 2.12 -13.58 ng L-1 naproxen, 15.74-18.74 ng L-1 salicylic acid and 5.8-121.2 ng L-1 caffeine.</p>


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