The hollow fiber liquid-phase microextraction allows highly selective concentration of organic compounds that are at trace levels. The determination of those analytes through the supercritical fluid chromatography usage is associated with many analytical benefits, which are significantly increased when it is coupled to a mass spectrometry detector, thus providing an extremely sensitive analytical technique with minimal consumption of organic solvents. On account of this, a hollow fiber liquid-phase microextraction technique in two-phase mode combined with supercritical fluid chromatography coupled to mass spectrometry was developed for quantifying 19 multiclass emerging contaminants in water samples in a total chromatographic time of 5.5 min. The analytical method used 40 μL of 1-octanol placed in the porous-walled polypropylene fiber as the acceptor phase, and 1 L of water sample was the donor phase. After extraction and quantification techniques were optimized in detail, a good determination coefficient (r2 > 0.9905) in the range of 0.1 to 100 μg L−1, for most of the analytes, and an enrichment factor in the range of 7 to 28,985 were obtained. The recovery percentage (%R) and intraday precision (%RSD) were in the range of 80.80–123.40%, and from 0.48 to 16.89%, respectively. Limit of detection and quantification ranged from 1.90 to 35.66 ng L−1, and from 3.41 to 62.11 ng L−1, respectively. Finally, the developed method was successfully used for the determination of the 19 multiclass emerging contaminants in superficial and wastewater samples.
This is a preview of subscription content, access via your institution.
Buy single article
Instant access to the full article PDF.
Tax calculation will be finalised during checkout.
Subscribe to journal
Immediate online access to all issues from 2019. Subscription will auto renew annually.
Tax calculation will be finalised during checkout.
Ramírez-Malule H, Quiñones-Murillo DH, Manotas-Duque D. Emerging contaminants as global environmental hazards. A bibliometric analysis. Emerg Contam. 2020;6:179–93. https://doi.org/10.1016/j.emcon.2020.05.001.
Richardson SD, Kimura SY. Emerging environmental contaminants: challenges facing our next generation and potential engineering solutions. Environ Technol Innov. 2017;8:40–56. https://doi.org/10.1016/j.eti.2017.04.002.
Peña-Guzmán C, Ulloa-Sánchez S, Mora K, Helena-Bustos R, Lopez-Barrera E, Alvarez J, et al. Emerging pollutants in the urban water cycle in Latin America: a review of the current literature. J Environ Manag. 2019;237:408–23. https://doi.org/10.1016/j.jenvman.2019.02.100.
Bieber S, Greco G, Grosse S, Letzel T. RPLC-HILIC and SFC with mass spectrometry: polarity-extended organic molecule screening in environmental (water) samples. Anal Chem. 2017;89:7907–14. https://doi.org/10.1021/acs.analchem.7b00859.
Kim K-H, Kabir E, Jahan SA. Exposure to pesticides and the associated human health effects. Sci Total Environ. 2016;575:525–35. https://doi.org/10.1016/j.scitotenv.2016.09.009.
de Souza RM, Seibert D, Quesada HB, de Jesus Bassetti F, Fagundes-Klen MR, Bergamasco R. Occurrence, impacts and general aspects of pesticides in surface water: a review. Process Saf Environ Prot. 2020;135:22–37. https://doi.org/10.1016/j.psep.2019.12.035.
Rice J, Lubben A, Kasprzyk-Hordern B. A multi-residue method by supercritical fluid chromatography coupled with tandem mass spectrometry method for the analysis of chiral and non-chiral chemicals of emerging concern in environmental samples. Anal Bioanal Chem. 2020;412:5563–81. https://doi.org/10.1007/s00216-020-02780-9.
Kharbouche L, Gil García MD, Lozano A, Hamaizi H, Galera MM. Solid phase extraction of pesticides from environmental waters using an MSU-1 mesoporous material and determination by UPLC-MS/MS. Talanta. 2019;199:612–9. https://doi.org/10.1016/j.talanta.2019.02.092.
Lopes D, Dias AN, Merib J, Carasek E. Hollow-fiber renewal liquid membrane extraction coupled with 96-well plate system as innovative high-throughput configuration for the determination of endocrine disrupting compounds by high-performance liquid chromatography-fluorescence and diode array de. Anal Chim Acta. 2018;1040:33–40. https://doi.org/10.1016/j.aca.2018.07.032.
Benedetti B, Majone M, Cavaliere C, Montone CM, Fatone F, Frison N, et al. Determination of multi-class emerging contaminants in sludge and recovery materials from waste water treatment plants: development of a modified QuEChERS method coupled to LC–MS/MS. Microchem J. 2020;155:104732. https://doi.org/10.1016/j.microc.2020.104732.
Arismendi D, Becerra-Herrera M, Cerrato I, Richter P. Simultaneous determination of multiresidue and multiclass emerging contaminants in waters by rotating-disk sorptive extraction–derivatization-gas chromatography/mass spectrometry. Talanta. 2019;201:480–9. https://doi.org/10.1016/j.talanta.2019.03.120.
García-Córcoles MT, Rodríguez-Gómez R, de Alarcón-Gómez B, Çipa M, Martín-Pozo L, Kauffmann JM, et al. Chromatographic methods for the determination of emerging contaminants in natural water and wastewater samples: a review. Crit Rev Anal Chem. 2019;49:160–86. https://doi.org/10.1080/10408347.2018.1496010.
Pano-Farias NS, Ceballos-Magaña SG, Gonzalez J, Jurado JM, Muñiz-Valencia R. Supercritical fluid chromatography with photodiode array detection for pesticide analysis in papaya and avocado samples. J Sep Sci. 2015;38:1240–7. https://doi.org/10.1002/jssc.201401174.
West C. Current trends in supercritical fluid chromatography. Anal Bioanal Chem. 2018;410:6441–57. https://doi.org/10.1007/s00216-018-1267-4.
Salvatierra-stamp V, Muñiz-Valencia R, Jurado JM, Ceballos-Magaña SG. Hollow fiber liquid phase microextraction combined with liquid chromatography-tandem mass spectrometry for the analysis of emerging contaminants in water samples. Microchem J. 2018;140. https://doi.org/10.1016/j.microc.2018.04.012.
Pilařová V, Plachká K, Khalikova MA, Svec F, Nováková L. Recent developments in supercritical fluid chromatography – mass spectrometry: is it a viable option for analysis of complex samples? TrAC Trends Anal Chem. 2019;112:212–25. https://doi.org/10.1016/j.trac.2018.12.023.
Liang Y, Zhou T. Recent advances of online coupling of sample preparation techniques with ultra high performance liquid chromatography and supercritical fluid chromatography. J Sep Sci. 2019;42:226–42. https://doi.org/10.1002/jssc.201800721.
He PX, Zhang Y, Zhou Y, Li GH, Zhang JW, Feng XS. Supercritical fluid chromatography-a technical overview and its applications in medicinal plant analysis: an update covering 2012-2018. Analyst. 2019;144:5324–52. https://doi.org/10.1039/c9an00826h.
Saito M. History of supercritical fluid chromatography: instrumental development. J Biosci Bioeng. 2013;115:590–9. https://doi.org/10.1016/j.jbiosc.2012.12.008.
Guillarme D, Desfontaine V, Heinisch S, Veuthey JL. What are the current solutions for interfacing supercritical fluid chromatography and mass spectrometry? J Chromatogr B Anal Technol Biomed Life Sci. 2018;1083:160–70. https://doi.org/10.1016/j.jchromb.2018.03.010.
Jalili V, Barkhordari A, Ghiasvand A. New extraction media in microextraction techniques. A review of reviews. Microchem J. 2020;153:104386. https://doi.org/10.1016/j.microc.2019.104386.
Carasek E, Morés L, Merib J. Basic principles, recent trends and future directions of microextraction techniques for the analysis of aqueous environmental samples. Trends Environ Anal Chem. 2018;19. https://doi.org/10.1016/j.teac.2018.e00060.
Carabajal M, Teglia CM, Cerutti S, Culzoni MJ, Goicoechea HC. Applications of liquid-phase microextraction procedures to complex samples assisted by response surface methodology for optimization. Microchem J. 2020;152:104436. https://doi.org/10.1016/j.microc.2019.104436.
Basheer C, Kamran M, Ashraf M, Lee HK. Enhancing liquid-phase microextraction efficiency through chemical reactions. TrAC Trends Anal Chem. 2019;118:426–33. https://doi.org/10.1016/j.trac.2019.05.049.
Rutkowska M, Płotka-Wasylka J, Sajid M, Andruch V. Liquid–phase microextraction: a review of reviews. Microchem J. 2019;149. https://doi.org/10.1016/j.microc.2019.103989.
Ghambarian M, Yamini Y, Esrafili A. Developments in hollow fiber based liquid-phase microextraction: principles and applications. Microchim Acta. 2012;177:271–94. https://doi.org/10.1007/s00604-012-0773-x.
Prosen H. Applications of hollow-fiber and related microextraction techniques for the determination of pesticides in environmental and food samples—a mini review. Separations. 2019;6:1–24. https://doi.org/10.3390/separations6040057.
Alsharif AMA, Tan GH, Choo YM, Lawal A. Efficiency of hollow fiber liquid-phase microextraction chromatography methods in the separation of organic compounds: a review. J Chromatogr Sci. 2017;55:378–91. https://doi.org/10.1093/chromsci/bmw188.
Jumhawan U, Bamba T. Green separation techniques for -omics platforms: supercritical fluid chromatography: Elsevier; 2020. https://doi.org/10.1016/b978-0-08-100596-5.22823-0.
Chen L, Dean B, La H, Chen Y, Liang X. Stereoselective supercritical fluidic chromatography –mass spectrometry (SFC-MS) as a fast bioanalytical tool to assess chiral inversion in vivo and in vitro. Int J Mass Spectrom. 2019;444:116172. https://doi.org/10.1016/j.ijms.2019.06.008.
Secretaría de Economía, Proyecto De Norma Mexicana Proy-Nmx-Aa-121/1-Scfi-2008 Análisis De Agua - Aguas Naturales Epicontinentales, Costeras Y Marinas – Muestreo - (Todas Las Partes Cancelan Al Proy Nmx-Aa-121-Scfi-2006) Water. 2008.
ICH. Guidance for industry Q2B validation of analytical procedures: methodology. 1996.
Commission of European-Communities. Council Directive 2002/657/EC concerning the performance of analytical methods and the interpretation of results. Off J Eur Communities. 2002:8–36.
Kokosa JM. Selecting an extraction solvent for a greener liquid phase microextraction (LPME) mode-based analytical method. TrAC Trends Anal Chem. 2019;118:238–47. https://doi.org/10.1016/j.trac.2019.05.012.
Valenzuela EF, Menezes HC, Cardeal ZL. New passive sampling device for effective monitoring of pesticides in water. Anal Chim Acta. 2019;1054:26–37. https://doi.org/10.1016/j.aca.2018.12.017.
Schulze S, Paschke H, Meier T, Muschket M, Reemtsma T, Berger U. A rapid method for quantification of persistent and mobile organic substances in water using supercritical fluid chromatography coupled to high-resolution mass spectrometry. Anal Bioanal Chem. 2020;412:4941–52. https://doi.org/10.1007/s00216-020-02722-5.
Salvatierra-Stamp thanks CONACYT for the grant provided. This work was also supported by the Red Temática de Toxicología de Plaguicidas-CONACYT.
Conflict of interest
The authors declare no conflict of interest.
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
About this article
Cite this article
Salvatierra-Stamp, V., Ceballos-Magaña, S.G., Pano-Farias, N.S. et al. Hollow fiber liquid-phase microextraction combined with supercritical fluid chromatography coupled to mass spectrometry for multiclass emerging contaminant quantification in water samples. Anal Bioanal Chem (2021). https://doi.org/10.1007/s00216-021-03202-0
- Multiclass emerging contaminants
- Hollow fiber liquid-phase microextraction
- Supercritical fluid chromatography
- Water samples