Abstract
A new sol–gel hybrid methyltrimethoxysilane–mercaptopropyltrimethoxysilane (MTMOS–MPTMS) was synthesized, characterized and applied as sorbent for solid phase extraction (SPE) of selected non-steroidal anti-inflammatory drugs (NSAIDs) as target analytes. Analysis was performed using high performance liquid chromatography with UV detection at 234 nm. Under the optimum extraction conditions (100 mg sorbent, 20 mL sample loading volume and 7 mL acetonitrile as desorption eluent), the method using the sol–gel organic–inorganic hybrid MTMOS–MPTMS as SPE sorbent showed good linearity in the range of 1–550 μg L−1, good repeatability (RSD 1.4–6.0 %, n = 3), low limits of detection at S/N = 3 (0.10–0.29 μg L−1) and limit of quantification (0.33–0.89 μg L−1, S/N = 10). The developed MTMOS–MPTMS SPE method was successfully applied to real sample analysis of the selected NSAIDs from several water samples. In-house MTMOS–MPTMS sol–gel hybrid material was able to extract the selected NSAIDs (diclofenac sodium, ketoprofen, mefenamic acid) in water samples comparable to commercial cyano sorbent. Excellent relative recoveries (RR) and RSDs of the NSAIDs were obtained from the various water samples (RR: 85.8–104.2 %, RSDs 1.2–6.0 %, n = 3) using the MTMOS–MPTMS SPE sorbent. The sol–gel hybrid MTMOS–MPTMS SPE sorbent demonstrates promising potential as an alternative inexpensive extraction sorbent for NSAIDs from water samples and with higher selectivity.
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References
Larsson N, Petersson E, Rylander M, Jonsson JA (2009) Continuous flow hollow fiber liquid-phase microextraction and monitoring of NSAID pharmaceuticals in a sewage treatment plant effluent. Anal Methods 1:59–67
Gallo P, Fabbrocino S, Vinci F, Fiori M, Danese V, Nasi A, Serpe L (2006) Multi-residue determination of non-steroidal anti-inflammatory drug residues in animal serum and plasma by HPLC and photo-diode array detection. J Chromatogr Sci 44:585–590
Fan W, Mao X, He M, Chen B (2014) Development of novel sol–gel coatings by chemically bonded ionic liquids for stir bar sorptive extraction—application for the determination of NSAIDS in real samples. Anal Bioanal Chem 406:7261–7273
Payan MR, Angel M, Lopez B, Torres RF, Bernal LP, Mochon MC (2009) Analytica chimica acta HPLC determination of ibuprofen, diclofenac and salicylic acid using hollow fiber-based liquid phase microextraction (HF-LPME). Anal Chim Acta 653:184–190
FDA-CDER (1998) Guidance for industry-environmental assessment of human drugs and biologics applications, Revision 1. FDA Centre for Drug Evaluation and Research, Rockville
Sebok A, Vasanits-Zsigrai A, Gy Palko, Gy Zaray, Molnar-Perl I (2008) Identification and quantification of ibuprofen, naproxen, ketoprofen and diclofenac present in waste-waters, as their trimethylsilyl derivatives, by gas chromatography mass spectrometry. Talanta 76:642–650
Arroyo D, Ortiz MC, Sarabia LA (2011) Optimization of the derivatization reaction and the solid-phase microextraction conditions using a D-optimal design and three-way calibration in the determination of non-steroidal anti-inflammatory drugs in bovine milk by gas chromatography–mass spectrometry. J Chromatogr A 1218:4487–4497
Galuszka A, Migaszewski Z, Namiesnik J (2012) Analytical Eco-Scale for assessing the greenness of analytical procedures. Trends Anal Chem 50:78–84
Van Aken K, Strekowski L, Patiny L (2006) EcoScale, a semi-quantitative tool to select an organic preparation based on economical and ecological parameters. Beilstein J Org Chem 2:1–7
Shen Y, Wu T, Zhang Y, Li J (2005) Comparison of two-typed (3-mercaptopropyl)trimethoxysilane-based networks on Au substrates. Talanta 65:481–488
Gomes Costa Silva R, Rosa Morais Vigna C, Bottoli CB, Collins CH, Agusto F (2010) Molecularly imprinted silica as a selective SPE sorbent for triazine herbicides. J Sep Sci 33:1319–1324
Bunch DR, Wang S (2013) Applications of monolithic solid-phase extraction in chromatography-based clinical chemistry assays. Anal Bioanal Chem 405:3021–3033
Wan Ibrahim WA, Farhani H, Sanagi MM, Aboul-Enein HY (2010) Solid phase microextraction using new sol–gel hybrid polydimethylsiloxane-2-hydroxymethyl-18-crown-6-coated fiber for determination of organophosphorous pesticides. J Chromatogr A 1217:4890–4897
Wan Ibrahim WA, Veloo KV, Sanagi MM (2012) Novel sol–gel hybrid methyltrimethoxysilane–tetraethoxysilane as solid phase extraction sorbent for organophosphorus pesticides. J Chromatogr A 1229:55–62
Sotoudehnia Korrani Z, Wan Ibrahim WA, Rashidi Nodeh H, Aboul-Enein HY, Sanagi MM (2015) Simultaneous preconcentration of polar and non-polar organophosphorus pesticides from water samples by using a new sorbent based on mesoporous silica. J Sep Sci. doi:10.1002/jssc.201500896
Belleville P (2010) Functional coatings: the sol–gel approach. C R Chim 13:97–105
Sarafraz-yazdi A, Abbasian M, Amiri A (2012) Determination of furan in food samples using two solid phase microextraction fibers based on sol–gel technique with gas chromatography–flame ionisation detector. Food Chem 131:698–704
Rashidi Nodeh H, Wan Ibrahim WA, Kamboh MA, Sanagi MM (2015) Dispersive graphene-based silica coated magnetic nanoparticles as a new adsorbent for preconcentration of chlorinated pesticides from environmental water. RSC Adv 5:76424–76434
Ali Omar MM, Wan Ibrahim WA, Elbashir AA (2014) Sol–gel hybrid methyltrimethoxysilane–tetraethoxysilane as a new dispersive solid-phase extraction material for acrylamide determination in food with direct gas chromatography–mass spectrometry analysis. Food Chem 158:302–309
Bagheri H, Aghakhani A, Es-haghi A (2007) Sol–gel-based SPME and GC–MS for trace determination of geosmin in water and apple juice samples. Chromatographia 66:779–783
Wan Ibrahim WA, Abdul Keyon AS, Prastomo N, Atsunori M (2011) Synthesis and characterization of polydimethylsiloxane–cyanopropyltriethoxysilane-derived hybrid coating for stir bar sorptive extraction. J Sol Gel–Sci Technol 59:128–134
Wan Ibrahim WA, Wan Ismail WN, Abdul Keyon AS, Sanagi MM (2011) Preparation and characterization of a new sol–gel hybrid based tetraethoxysilane–polydimethylsiloxane as a stir bar extraction sorbent materials. J Sol–Gel Sci Technol 58:602–611
Zhou L, Kong Y, Zhong S, Zhou X (2013) Preparation and characterization of molecularly imprinted organic–inorganic hybrid materials by sol–gel processing for selective recognition of ibuprofen. J Sol–Gel Sci Technol 66:59–67
Huang H, Orler B, Wilkes GL, Materials P (1985) Ceramers: hybrid materials incorporating polymeric/oligomeric species with inorganic glasses by a sol–gel process. Polym Bull 564:557–564
Ali I, Kulsum U, AL-Othman ZA, Saleem K (2016) Analyses of nonsteroidal anti-inflammatory drugs in human plasma using dispersive nano solid-phase extraction and high-performance liquid chromatography. Chromatographia 79:145–157
Shaaban H, Gorecki T (2011) High temperature–high efficiency liquid chromatography using sub-2 µm coupled columns for the analysis of selected non-steroidal anti-inflammatory drugs and veterinary antibiotics in environmental samples. Anal Chim Acta 702:136–143
Luo YB, Zheng HB, Wang JX, Gao Q, Yu QW, Feng YQ (2011) An anionic exchange stir rod sorptive extraction based on monolithic material for the extraction of non-steroidal anti-inflammatory drugs in environmental aqueous samples. Talanta 86:103–108
Sagrista E, Larsson E, Ezoddin M, Hidalgo M, Salvado V, Jonsson JA (2010) Determination on non-steroidal anti-inflammatory drugs in sewage sludge by direct hollow fiber support liquid microextraction and liquid chromatography–mass spectroscopy. J Chromatogr A 1217:6153–6158
Acknowledgments
This work was supported by grants from the Research University Grant (GUP) (Vote Numbers: 01H94, 04H22) and Ministry of Education Malaysia (MOHE). The Ministry of Education Malaysia (MOE) is acknowledged for My Brain 15 Fellowship (MyPhD) award to M. Abd Rahim.
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Abd Rahim, M., Wan Ibrahim, W.A., Ramli, Z. et al. New Sol–Gel Hybrid Material in Solid Phase Extraction Combined with Liquid Chromatography for the Determination of Non-steroidal Anti-inflammatory Drugs in Water Samples. Chromatographia 79, 421–429 (2016). https://doi.org/10.1007/s10337-016-3059-3
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DOI: https://doi.org/10.1007/s10337-016-3059-3