Flow injection photoinduced chemiluminescence determination of imazalil in water samples

The final publication is available at link.springer.com[EN] In this work, a fast, simple and economic method is proposed for the determination of imazalil in water samples by flow injection photoinduced chemiluminescence. In this method, imazalil degrades in basic media through the use of a photoreactor, and the resulting photofragments react with ferricyanide and generate the direct chemiluminescence signal. To the authors' knowledge, this is the first time that a chemiluminescence method has been proposed for the determination of this fungicide. All physical and chemical parameters in the flow injection chemiluminescence system were optimized in the experimental setting. In the absence of preconcentration, the linear dynamic range for imazalil was 0.75-5 mg L(-1) and the detection limit was 0.171 mg L(-1). The application of solid-phase extraction with C18 cartridges allowed the elimination of interference ions, the reduction of the linear dynamic range to 15-100 mu g L(-1), and a detection limit of 3.4 mu g L(-1). This detection limit is below the maximum concentration level established by the Regulations of the Hydraulic Public Domain for pesticide dumping. The sample throughput after solid-phase extraction of the analyte was 12 samples h(-1). The intraday and interday coefficients of variation were below 9.9% in all cases. This method was applied to the analysis of environmental water samples, and recoveries of between 95.7 and 110% were obtained.The authors are grateful to The Spanish Ministry of Education and Science and FEDER funds for financial support (project CTM2006-11991). The translation of this paper was funded by the Universidad Politécnica de Valencia, Spain.Meseguer-Lloret, S.; Torres-Cartas, S.; Gómez Benito, C. (2010). Flow injection photoinduced chemiluminescence determination of imazalil in water samples. Analytical and Bioanalytical Chemistry. 398(7-8):3175-3182. https://doi.org/10.1007/s00216-010-4227-1S317531823987-8EC (1998) Council Directive 98/83/EC of 3 November 1998 on the quality of water intended for human consumption. European Council, BrusselsSpanish Ministry of Public Works and Transportation (1986) Royal Decree 849/1986 of 11 April of the Regulations of the Hydraulic Public Domain. Spanish Ministry of Public Works and Transportation, MadridPicó Y, la Farré M, Soler C, Barceló D (2007) J Chromatogr A 1176(1-2):123–134Ibáñez M, Sancho JV, Hernández F, McMillan D, Rao R (2008) Trends Anal Chem 27(5):481–489Yoshioka N, Akiyama Y, Teranishi K (2004) J Chromatogr A 1022(1–2):145–150Watanabe E, Yoshimura Y, Yuasa Y, Nakazawa H (2001) Anal Chim Acta 433(2):199–206Ito Y, Ikai Y, Oka H, Hayakawa J, Kagami T (1998) J Chromatogr A 810(1-2):81–87Garrido J, de Alba M, Jimenez I, Casado E, Folgueiras ML (1997) J Chromatogr A 765(1):91–97Charlton AJA, Jones A (2007) J Chromatogr A 1141(1):117–122Rodríguez R, Picó Y, Font G, Mañes J (2001) J Chromatogr A 924(1-2):387–396Balinova A (1995) Anal Chim Acta 311(3):423–427Menezes Filho A, Neves dos Santos F, Afonso de Pereira P (2010) Mikrochemical J 96:139–145Beale DJ, Porter NA, Roddick FA (2009) Talanta 78(2):342–347Albert-García JR, Martínez-Calatayud J (2008) Talanta 75(3):717–724Meseguer-Lloret S, Campíns-Falcó P, Tortajada-Genaro LA, Blasco-Gómez F (2003) Int J Environ Anal Chem 83(5):405–416Moliner-Martínez Y, Meseguer-Lloret S, Tortajada-Genaro LA, Campíns-Falcó P (2003) Talanta 60(2-3):257–268Lin Q, Guiraúm A, Escobar R, de la Rosa F (1993) Anal Chim Acta 283(1):379–385Townshend A, Ruengsitagoon W, Thongpoon C, Liawruangrath S (2005) Anal Chim Acta 541:105–111Lattanzio G, García-Campaña AM, Soto-Chinchilla JJ, Gámiz-Gracia L, Girotti S (2008) J Pharm Biomed Anal 46(2):381–385Catalá Icardo M, García Mateo JV, Fernández Lozano M, Martínez Calatayud J (2003) Anal Chim Acta 499(1-2):57–69Ciborowski M, Catalá Icardo M, García Mateo JV, Martínez Calatayud J (2004) J Pharm Biomed Anal 36(4):693–700Yang XF, Li H (2004) Talanta 64(2):478–483Gómez-Taylor B, Palomeque M, García Mateo JV, Martínez Calatayud J (2006) J Pharm Biomed Anal 41(2):347–357López Paz JL, Catalá-Icardo M (2008) Anal Chim Acta 625(2):173–179López Malo D, Martínez Calatayud J (2008) Talanta 77(2):561–56

Selective and sensitive chemiluminescence determination of MCPB: flow injection and liquid chromatography

This paper was published in Applied Spectroscopy and is made available as an electronic reprint with the permission of OSA. The paper can be found at the following URL on the OSA website: http://dx.doi.org/10.1177/0003702815620133 . Systematic or multiple reproduction or distribution to multiple locations via electronic or other means is prohibited and is subject to penalties under law.Two new chemiluminescence (CL) methods are described for the determination of the herbicide 4-(4-chloro-o-tolyloxy) butyric acid (MCPB). First, a flow injection chemiluminescence (FI-CL) method is proposed. In this method, MCPB is photodegraded with an ultraviolet (UV) lamp and the photoproducts formed provide a great CL signal when they react with ferricyanide in basic medium. Second, a high-performance liquid chromatography chemiluminescence (HPLC-CL) method is proposed. In this method, before the photodegradation and CL reaction, the MCPB and other phenoxyacid herbicides are separated in a C18 column. The experimental conditions for the FI-CL and HPLC-CL methods are optimized. Both methods present good sensitivity, the detection limits being 0.12 mg L 1 and 0.1 mg L 1 (for FI-CL and HPLC-CL, respectively) when solid phase extraction (SPE) is applied. Intra- and interday relative standard deviations are below 9.9%. The methods have been satisfactorily applied to the analysis of natural water samples. FI-CL method can be employed for the determination of MCPB in simple water samples and for the screening of complex water samples in a fast, economic, and simple way. The HPLC-CL method is more selective, and allows samples that have not been resolved with the FI-CL method to be solved.Meseguer-Lloret, S.; Torres-Cartas, S.; Catalá-Icardo, M.; Gómez Benito, C. (2016). Selective and sensitive chemiluminescence determination of MCPB: flow injection and liquid chromatography. Applied Spectroscopy. 70(2):312-321. doi:10.1177/0003702815620133S312321702Moral, A., Caballo, C., Sicilia, M. D., & Rubio, S. (2012). Highly efficient microextraction of chlorophenoxy acid herbicides in natural waters using a decanoic acid-based nanostructured solvent prior to their quantitation by liquid chromatography–mass spectrometry. Analytica Chimica Acta, 709, 59-65. doi:10.1016/j.aca.2011.10.016Herrero-Hernández, E., Rodríguez-Gonzalo, E., Andrades, M. S., Sánchez-González, S., & Carabias-Martínez, R. (2013). Occurrence of phenols and phenoxyacid herbicides in environmental waters using an imprinted polymer as a selective sorbent. Science of The Total Environment, 454-455, 299-306. doi:10.1016/j.scitotenv.2013.03.029Baggiani, C., Giovannoli, C., Anfossi, L., & Tozzi, C. (2001). Molecularly imprinted solid-phase extraction sorbent for the clean-up of chlorinated phenoxyacids from aqueous samples. Journal of Chromatography A, 938(1-2), 35-44. doi:10.1016/s0021-9673(01)01126-8Wintersteiger, R., Goger, B., & Krautgartner, H. (1999). Quantitation of chlorophenoxy acid herbicides by high-performance liquid chromatography with coulometric detection. Journal of Chromatography A, 846(1-2), 349-357. doi:10.1016/s0021-9673(99)00429-xPeruzzi, M., Bartolucci, G., & Cioni, F. (2000). Determination of phenoxyalkanoic acids and other herbicides at the ng/ml level in water by solid-phase extraction with poly(divinylbenzene-co-N-vinylpyrrolidone) sorbent and high-performance liquid chromatography–diode-array detection. Journal of Chromatography A, 867(1-2), 169-175. doi:10.1016/s0021-9673(99)01141-3Ranz, A., & Lankmayr, E. (2006). Screening and optimization of the derivatization of polar herbicides with trimethylanilinium hydroxide for GC-MS analysis. Journal of Biochemical and Biophysical Methods, 69(1-2), 3-14. doi:10.1016/j.jbbm.2006.02.007Nuhu, A. A., Basheer, C., Alhooshani, K., & Al-Arfaj, A. R. (2012). Determination of phenoxy herbicides in water samples using phase transfer microextraction with simultaneous derivatization followed by GC-MS analysis. Journal of Separation Science, 35(23), 3381-3388. doi:10.1002/jssc.201200218Jiménez, J. J. (2013). Simultaneous liquid–liquid extraction and dispersive solid-phase extraction as a sample preparation method to determine acidic contaminants in river water by gas chromatography/mass spectrometry. Talanta, 116, 678-687. doi:10.1016/j.talanta.2013.07.052EREMIN, S., LAASSIS, B., & AARON, J. (1996). Photochemical-fluorimetric method for the determination of total chlorophenoxyacid herbicides. Talanta, 43(3), 295-301. doi:10.1016/0039-9140(95)01751-8Jafari, M. T., Saraji, M., & Yousefi, S. (2012). Negative electrospray ionization ion mobility spectrometry combined with microextraction in packed syringe for direct analysis of phenoxyacid herbicides in environmental waters. Journal of Chromatography A, 1249, 41-47. doi:10.1016/j.chroma.2012.06.024Tsogas, G. Z., Giokas, D. L., Nikolakopoulos, P. G., Vlessidis, A. G., & Evmiridis, N. P. (2006). Determination of the pesticide carbaryl and its photodegradation kinetics in natural waters by flow injection–direct chemiluminescence detection. Analytica Chimica Acta, 573-574, 354-359. doi:10.1016/j.aca.2005.11.058Albert-García, J. R., & Calatayud, J. M. (2008). Determination of the herbicide benfuresate by its photo-induced chemiluminescence using flow multicommutation methodology. Talanta, 75(3), 717-724. doi:10.1016/j.talanta.2007.12.003Catalá-Icardo, M., López-Paz, J. L., Choves-Barón, C., & Peña-Bádena, A. (2012). Native vs photoinduced chemiluminescence in dimethoate determination. Analytica Chimica Acta, 710, 81-87. doi:10.1016/j.aca.2011.10.043Gómez-Benito, C., Meseguer-Lloret, S., & Torres-Cartas, S. (2013). Sensitive determination of Fenamiphos in water samples by flow injection photoinduced chemiluminescence. International Journal of Environmental Analytical Chemistry, 93(2), 152-165. doi:10.1080/03067319.2012.663755Beale, D. J., Porter, N. A., & Roddick, F. A. (2009). A fast screening method for the presence of atrazine and other triazines in water using flow injection with chemiluminescent detection. Talanta, 78(2), 342-347. doi:10.1016/j.talanta.2008.11.033Catalá-Icardo, M., López-Paz, J. L., & Pérez-Plancha, L. M. (2014). Fast Determination of Thiacloprid by Photoinduced Chemiluminescence. Applied Spectroscopy, 68(6), 642-648. doi:10.1366/13-07330Torres-Cartas, S., Gómez-Benito, C., & Meseguer-Lloret, S. (2011). FI on-line chemiluminescence reaction for determination of MCPA in water samples. Analytical and Bioanalytical Chemistry, 402(3), 1289-1296. doi:10.1007/s00216-011-5567-1Catalá-Icardo, M., Lahuerta-Zamora, L., Torres-Cartas, S., & Meseguer-Lloret, S. (2014). Determination of organothiophosphorus pesticides in water by liquid chromatography and post-column chemiluminescence with cerium(IV). Journal of Chromatography A, 1341, 31-40. doi:10.1016/j.chroma.2014.03.024Huertas-Pérez, J. F., & García-Campaña, A. M. (2008). Determination of N-methylcarbamate pesticides in water and vegetable samples by HPLC with post-column chemiluminescence detection using the luminol reaction. Analytica Chimica Acta, 630(2), 194-204. doi:10.1016/j.aca.2008.09.047Orejuela, E., & Silva, M. (2003). Monitoring some phenoxyl-type N-methylcarbamate pesticide residues in fruit juices using high-performance liquid chromatography with peroxyoxalate-chemiluminescence detection. Journal of Chromatography A, 1007(1-2), 197-201. doi:10.1016/s0021-9673(03)00934-8GALERA, M., GARCIA, M., & VALVERDE, R. (2008). Determination of photoirradiated high polar benzoylureas in tomato by HPLC with luminol chemiluminescence detection. Talanta, 76(4), 815-823. doi:10.1016/j.talanta.2008.04.052Rosales-Conrado, N., León-González, M. E., Pérez-Arribas, L. V., & Polo-Díez, L. M. (2005). Effect of temperature on the separation of chlorophenoxy acids and carbamates by capillary high-performance liquid chromatography and UV (or diode array) detection. Journal of Chromatography A, 1081(1), 114-121. doi:10.1016/j.chroma.2004.12.083Geerdink, R. B., van Tol-Wildenburg, S., Niessen, W. M. A., & Brinkman, U. A. T. (1997). Determination of Phenoxy Acid Herbicides From Aqueous Samples by Improved Clean-up on Polymeric Pre-columns at High pH. The Analyst, 122(9), 889-894. doi:10.1039/a702338

Determination of organothiophosphorus pesticides in water by liquid chromatography and post-column chemiluminescence with cerium(IV)

A new, fast, selective and sensitive method has been developed for the simultaneous determination of nine organothiophosphorus (OTP) pesticides, namely omethoate, dimethoate, disulfoton-sulfoxide, methidathion, phosmet, malathion, diazinon, pirimiphos-methyl and chlorpyrifos. The pesticides were separated on a Kinetex C18 column by gradient elution with acetonitrile:water. A post-column basic hydrolysis of the pesticides and later a chemiluminescence (CL) reaction with cerium (IV) in acid medium was carried out. Hexadecylpyridinium chloride highly enhanced the CL emission. Under optimized conditions, linearity, precision, limits of detection and quantification, and accuracy were determined. Both selectivity and sensitivity were compared with those obtained with UV detection. In combination with SPE, limits of detection in the range 15-80 ng/L and 5-30 ng/L were obtained when 250 mL and 1000 mL of solution were treated, respectively. When applied to 250 mL of sample the inter-day precision of the method was between 3.5% and 7.3% and the intra-day precision between 2.9% and 6.0%. The method was applied to determine OTP pesticides in spiked water samples from different origins: irrigation, river, sea, ground, spring, mineral and tap waters, being the percentage of recovery of added amounts near 100% form most of the pesticides.Catalá Icardo, M.; Lahuerta Zamora, L.; Torres-Cartas, S.; Meseguer-Lloret, S. (2014). Determination of organothiophosphorus pesticides in water by liquid chromatography and post-column chemiluminescence with cerium(IV). Journal of Chromatography A. 1341:31-40. doi:10.1016/j.chroma.2014.03.0243140134

A guide to avoid method bias of chromium(III, VI) chemiluminescence determination by luminol-hydrogen peroxide reaction. Application to unknown water samples

This is an Author's Accepted Manuscript of an article published in International Journal of Environmental & Analytical Chemistry, 83, 5, 405-416. DOI: 10.1080/0306731031000101383 © Taylor & Francis, available online at: http://doi.org/10.1080/0306731031000101383[EN] Cr(III) and/or Cr(VI) determinations based on light emission produced by luminol oxidation by hydrogen peroxide in basic aqueous solution catalyzed by Cr(III) were studied in order to diagnose and/or avoid method bias. The calibration step was optimized, and the usefulness of the method for speciating chromium was tested. The use of the standard addition method in the linear interval concentration range made it possible to diagnose the accuracy of the method for real samples. Good results were obtained for several real water samples containing chromium at different concentrations. The proposed protocol made the method traceable with an appropriate certified reference material and with the reference method.The authors are grateful to the DGICYT (Project n PB 97-1387) and to the Generalitat Valenciana (GR-0036) for financial support.Meseguer-Lloret, S.; Campins-Falcó, P.; Tortajada-Genaro, LA.; Blasco-Gómez, F. (2003). A guide to avoid method bias of chromium(III, VI) chemiluminescence determination by luminol-hydrogen peroxide reaction. Application to unknown water samples. International Journal of Environmental & Analytical Chemistry. 83(5):405-416. https://doi.org/10.1080/0306731031000101383S40541683

Multivariate calibration applied to simultaneous chemiluminiscence determination of Cobalt and Chromium

The final publication is available at http://doi.org/ 10.1007/s00216-002-1637-8[EN] The simultaneous determination of chromium and cobalt in water samples has been studied. Chemiluminescence registers based on the luminol-hydrogen peroxide reaction have obtained by a batch procedure. PLS algorithms have employed to model the time-response (formation and destruction of emitter). The influence of the presence of two metals and the non-linearity relationship between response and concentration have been evaluated in the signal. Different experimental designs and the selection of variables have been tested. The calibration set has been selected based on two criteria: unicomponent and/or bicomponent standard solutions and the slope calculated from linear univariate calibration. The response has been modelled providing high percentages of explained variance, robust models and low prediction errors. The proposed methodology has been validated using test standard solutions and a standard reference material of fresh water. Accurate results have proved the advantages of this method for the simultaneous determination of chromium and cobalt in water samples.The authors are grateful to the DGICYT (Project no PB 97–1387) for financial support. S.M.Ll. and L.A.T.G. express their gratitude to Ministerio de Educación y Cultura (Spain) for the predoctoral grant.Campins-Falcó, P.; Tortajada-Genaro, LA.; Meseguer-Lloret, S.; Bosch-Reig, F. (2002). Multivariate calibration applied to simultaneous chemiluminiscence determination of Cobalt and Chromium. Analytical and Bioanalytical Chemistry. 374(7-8):1223-1229. https://doi.org/10.1007/s00216-002-1637-8S122312293747-

Influence of water sample storage protocols in chemiluminescence detection of trace elements by batch or FI modes

[EN] This paper shows the influence of different sample storage protocols, on the chemiluminescence signal of some metal ions. The storage protocols studied were: acid addition (HCl or HNO3) and no reagent addition to filtered and refrigerated (T=4 °C) samples. Light emission was produced for the chemiluminescence reaction between luminol and hydrogen peroxide in buffer carbonate conditions (pH 10.8) catalysed by Cr(III), Co(II) and Cu(II). Batch and/or flow modes in different conditions were tested. Fe(II), Fe(III), Ni(II) and Mn(II) did not give chemiluminescence in the studied conditions. A parallel study of sensitivity and selectivity was performed. Then the presence or absence of the masking agent EDTA, added to samples or used in the carrier stream, is assayed. If the samples are acidified with HNO3, a previous neutralisation is needed using batch mode. The determination of Cr(III) is independent of storage protocol by flow injection (FI) method; however, the determination of Co(II) or Cu(II) or total determination of three metals requires the conditioning of standards. Detection limits achieved are ranged between 0.5 and 2 ¿g l¿1. For batch mode, detection limits are better for unacidified samples and worse for carbonate-neutralised samples. The influence of storage protocols was validated using standard metal mixtures and calibration solutions. The use of standard reference material (SRM© 1640) (Trace elements in natural water) corroborates the previous statements and validates the accuracy of the different approaches underlined. This paper demonstrates that it is possible to determine Cr(III) selectively in natural waters.The authors are grateful to the DGICYT (Project No. PB 97-1387) for financial support. Y.M.M., S.M.L. and L.A.T.G. express their gratitude to Ministerio de Educación y Cultura (Spain) for the predoctoral grant.Molliner Martínez, Y.; Meseguer-Lloret, S.; Tortajada-Genaro, LA.; Campins-Falcó, P. (2003). Influence of water sample storage protocols in chemiluminescence detection of trace elements by batch or FI modes. Talanta. 60(1):257-268. https://doi.org/10.1016/S0039-9140(03)00068-7S25726860

Photografted fluoropolymers as novel chromatographic supports for polymeric monolithic stationary phases

[EN] In this study, porous polymer monoliths were in situ synthesized in fluoropolymers tubing to prepare microbore HPLC columns. To ensure the formation of robust homogeneous polymer monoliths in these housing supports, the inner surface of fluoropolymer tubing was modified in a two-step photografting process. Raman spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the inner poly(ethylene-co-tetrafluoroethylene) (ETFE) wall and the subsequent attachment of a monolith onto the wall. Poly(glycidyl methacrylate-co-divinylbenzene), poly(butyl methacrylate-co-ethyleneglycol dimethacrylate) and poly(styrene-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface vinylized ETFE tubes. The resulting monoliths exhibited good permeability and mechanical stability (pressure resistance up to 9¿MPa). The chromatographic performance of these different monolithic columns was evaluated via the separation of alkyl benzenes and proteins in a conventional HPLC system.This work was supported by project PROMETEO/2016/145 (Conselleria d'Educacio, Investigacio, Cultura i Esport,Esport, Generalitat Valenciana, Spain). The authors also thank Dr. S. Laredo-Ortiz from the Atomic Spectroscopy section of the SCSIE (University of Valencia), for her help in Raman measurements.Catalá-Icardo, M.; Torres-Cartas, S.; Meseguer-Lloret, S.; Simó-Alfonso, E.; Herrero Martínez, J. (2018). Photografted fluoropolymers as novel chromatographic supports for polymeric monolithic stationary phases. Talanta. 187:216-222. doi:10.1016/j.talanta.2018.05.026S21622218

Recent Advances in Molecularly Imprinted Membranes for Sample Treatment and Separation

[EN] This review describes the recent advances from the past five years concerning the development and applications of molecularly imprinted membranes (MIMs) in the field of sample treatment and separation processes. After a short introduction, where the importance of these materials is highlighted, a description of key aspects of membrane separation followed by the strategies of preparation of these materials is described. The review continues with several analytical applications of these MIMs for sample preparation as well as for separation purposes covering pharmaceutical, food, and environmental areas. Finally, a discussion focused on possible future directions of these materials in extraction and separation field is also given.This work was supported by project RTI2018-095536-B-I00 (Ministry of Science, Innovation and Universities, Spain).Torres-Cartas, S.; Catalá-Icardo, M.; Meseguer-Lloret, S.; Simó-Alfonso, EF.; Herrero-Martínez, JM. (2020). Recent Advances in Molecularly Imprinted Membranes for Sample Treatment and Separation. Separations. 7(4):1-28. https://doi.org/10.3390/separations7040069S1287

Extraction and preconcentration of organophosphorus pesticides in water by using a polymethacrylate-based sorbent modified with magnetic nanoparticles

[EN] A polymethacrylate-based sorbent modified with magnetic nanoparticles (MNPs) has been synthesized and used as sorbent for solid-phase extraction (SPE) and magnetic solid-phase extraction (MSPE) of three organophosphorus pesticides (phosmet, pirimiphos-methyl, and chlorpyrifos) in water samples followed by high-performance liquid chromatography diode array detection. The sorbent was prepared from a glycidyl methacrylate-based polymer, modified with a silanizing agent, followed by immobilization of MNPs on the surface of the material. The sorbent was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. Comparative studies of this support were done both in conventional SPE cartridge and MSPE approach. Several extraction parameters (loading pH, elution solvent, eluting volume, and loading flow rate) were investigated in detail. Under optimal conditions, the proposed sorbent gave an excellent enrichment efficiency of analytes and detection limits between 0.01 and 0.25 μg L−1. The recoveries of organophosphorus pesticides in spiked water samples were in the range of 71 98%, and the developed sorbent showed a high reusability (up to 50 uses without losses in recovery). The proposed method was satisfactorily applied to the analysis of these pesticides in water samples from different sources.This work was supported by projects CTQ2014-52765-R (MINECO of Spain and FEDER) and PROMETEO/2016/145 (Conselleria de Educacion, Investigacion, Cultura y Deporte of Generalitat Valenciana, Spain).Meseguer-Lloret, S.; Torres-Cartas, S.; Catalá-Icardo, M.; Simó-Alfonso, EF.; Herrero-Martínez, JM. (2017). Extraction and preconcentration of organophosphorus pesticides in water by using a polymethacrylate-based sorbent modified with magnetic nanoparticles. 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Polymer-based materials modified with magnetite nanoparticles for enrichment of phospholipids

[EN] A polymeric material modified with magnetic nanoparticles (MNPs) has been synthesized and evaluated as sorbent both for solid-phase extraction (SPE) and dispersive magnetic solid-phase extraction (MSPE) of phospholipids (PLs) in human milk samples. The synthesized sorbent was characterized by scanning electron microscopy and its iron content was also determined. Several experimental variables that affect the extraction performance (e.g. loading solvent, breakthrough volume and loading capacity) were investigated and a comparison between conventional SPE and MSPE modalities was done. The proposed method was satisfactorily applied to the analysis of PLs in human milk fat extracts in different lactation stages and the extracted PLs were determined by means of hydrophilic interaction liquid chromatography using evaporative light scattering detection.Project CTQ2017-84995-R (MINECO of Spain and FEDER) and PROMETEO/2016/145 (Generalitat Valenciana). I. T-D thanks the MINECO for an FPU grant for Ph,D. studies.Ten-Domenech. I.; Martínez-Pérez-Cejuela, H.; Simó-Alfonso, E.; Torres-Cartas, S.; Meseguer-Lloret, S.; Herrero Martínez, J. (2018). Polymer-based materials modified with magnetite nanoparticles for enrichment of phospholipids. Talanta. 180:162-167. https://doi.org/10.1016/j.talanta.2017.12.042S16216718