scholarly journals Fabrication of calixarene-grafted bio-polymeric magnetic composites for magnetic solid phase extraction of non-steroidal anti-inflammatory drugs in water samples

PeerJ ◽  
2018 ◽  
Vol 6 ◽  
pp. e5108 ◽  
Author(s):  
Syed Fariq Fathullah Syed Yaacob ◽  
Arniza Khairani Mohd Jamil ◽  
Muhammad Afzal Kamboh ◽  
Wan Aini Wan Ibrahim ◽  
Sharifah Mohamad

Calixarene framework functionalized bio-polymeric magnetic composites (MSp-TDI-calix) were synthesized and utilized as magnetic solid-phase extraction (MSPE) sorbent for the extraction of non-steroidal anti-inflammatory drugs (NSAIDs), namely indoprofen (INP), ketoprofen (KTP), ibuprofen (IBP) and fenoprofen (FNP), from environmental water samples. MSp-TDI-calix was characterized by FT-IR, XRD, FESEM, EDX, VSM and BET analysis, and the results were compared with Sp-TDI and Sp-TDI-calix. To maximize the extraction performance of MSp-TDI-calix decisive MSPE affective parameters such as sorbent amount, extraction time, sample volume, type of organic eluent, volume of organic eluent, desorption time and pH were comprehensively optimized prior to HPLC-DAD determination. The analytical validity of the proposed MSPE method was evaluated under optimized conditions and the following figures of merit were acquired: linearity with good determination coefficient (R2 ≥ 0.991) over the concentration range of 0.5–500 µg/L, limits of detection (LODs) ranged from 0.06–0.26 µg/L and limits of quantitation (LOQ) between 0.20–0.89 µg/L. Excellent reproducibility and repeatability under harsh environment with inter-day and intra-day relative standard deviations were obtained in the range of 2.5–3.2% and 2.4–3.9% respectively. The proposed method was successfully applied for analysis of NSAIDs in tap water, drinking water and river water with recovery efficiency ranging from 88.1–115.8% with %RSD of 1.6–4.6%.

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%).


2020 ◽  
Vol 59 (1) ◽  
pp. 95-102
Author(s):  
Dan-Dan Wang ◽  
Zhi-Heng Lu ◽  
Xiao-yu Guan ◽  
Mei-Nan Ou Yang ◽  
Hao-Ming Guo ◽  
...  

Abstract A novel magnetic solid-phase extraction technique coupled to ultraperformance liquid chromatography has been developed for separation and preconcentration of four sulfonylurea herbicides (sulfosulfuron, bensulfuron-methyl, pyrazosulfuron-ethyl and halosulfuro-methyl) in aqueous samples. The key point of this method was the application of a novel magnetic nanomaterial that composed of a low eutectic solvent as a shell coated on the magnetic core modified by polydopamine. The extensive active sites outside the low eutectic solvent can effectively adsorb the target herbicide in the extraction process. The obtained magnetic adsorbent was characterized with fourier transform infrared spectrometry, scanning electron microscopy and vibrating sample magnetometer. The influence parameters relevant to this method were optimized. Under the optimum conditions, good linearities could be obtained within the range of 1.0–200 μg L−1 for all analytes, with correlation coefficients ≥0.9908. The limit of detections of the method was between 0.0074 and 0.0100 μg L−1 and the relative standard deviations were 1.1–3.6%. The enrichment factor is 66.6. In the final experiment, the proposed method was successfully applied to the analysis of sulfonylurea herbicides residue in environment and drinking-water samples, and the obtained recoveries were between 70.6% and 109.4%.


2021 ◽  
Author(s):  
Hongmei Liu ◽  
Shihao Dang ◽  
Gu A ◽  
Baogui Ye

Good magnetic and rich interactions with targets for sorbent are important ways to improve its efficiency of magnetic solid-phase extraction (MSPE). Here, the magnetic MOF-101 derivative (MD) material is obtained...


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