Abstract
A procedure based on vortex-assisted matrix solid-phase dispersion (MSPD) for the extraction of 15 pharmaceuticals from fish samples with determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was validated. Florisil, C18, diatomaceous earth, chitin, and chitosan were evaluated as solid supports. Best results were obtained with 0.5 g of diatomaceous earth, 0.5 g of sodium sulfate, and 5 mL of methanol. Analytical recoveries ranged from 58 to 128 % with relative standard deviation (RSD) lower than 15 %. Limit of quantification (LOQ) values for the 15 compounds ranged from 5 to 1000 ng g−1. The method under investigation has shown to be a simple and fast extraction tool with minimum instrumentation and low amount of reagent, resulting in method low cost. Besides, alternative materials, such as chitin and chitosan, which were applied to the dispersion step for the first time, were found to be interesting alternatives.
Similar content being viewed by others
References
Petrovic M, Farre M, de Alda ML, Perez S, Postigo C, Kock M, Radjenovic J, Gros M, Barcelo D (2010) Recent trends in the liquid chromatography-mass spectrometry analysis of organic contaminants in environmental samples. J Chromatogr A 1217:4004–4017
Wille K, De Brabander HF, Vanhaecke L, De Wulf E, Van Caeter P, Janssen CR (2012) Coupled chromatographic and mass-spectrometric techniques for the analysis of emerging pollutants in the aquatic environment. TrAC Trend Anal Chem 35:87–108
Kosma CI, Lambropoulou LA, Albanis TA (2010) Occurrence and removal of PPCPs in municipal and hospital wastewaters in Greece. J Hazard Mater 179:804–817
Primel EG, Caldas SS, Escarrone ALV (2012) Multi-residue analytical methods for the determination of pesticides and PPCPs in water by LC-MS/MS: a review. Cent Euro J Chem 10:876–899
Dórea JG (2008) Persistent, bioaccumulative and toxic substances in fish: human health considerations. Sci Total Environ 400:93–114
Madureira TV, Rocha MJ, Cruzeiro C, Rodrigues I, Monteiro RA, Rocha E (2012) The toxicity potential of pharmaceuticals found in the Douro River estuary (Portugal): evaluation of impacts on fish liver, by histopathology, stereology, vitellogenin and CYP1A immunohistochemistry, after sub-acute exposures of the zebrafish model. Environ Toxicol Pharmacol 34:34–45
Gobas FAPC, Wilcockson JB, Russell RW, Haffner GD (1998) Mechanism of biomagnification in fish under laboratory and field conditions. Environ Sci Technol 33:133–141
Baird C, Cann M (2008) Química ambiental. Bookman
Hazelton PD, Cope WG, Mosher S, Pandolfo TJ, Belden JB, Barnhart MC, Bringolf RB (2013) Fluoxetine alters adult freshwater mussel behavior and larval metamorphosis. Sci Total Environ 445–446:94–100
Giltrow E, Eccles PD, Winter MJ, McCormack PJ, Rand-Weaver M, Hutchinson TH, Sumpter JP (2009) Chronic effects assessment and plasma concentrations of the beta-blocker propranolol in fathead minnows (Pimephales promelas). Aquat Toxicol 95:195–202
Oaks JL, Gilbert M, Virani MZ, Watson RT, Meteyer CU, Rideout BA, Shivaprasad HL, Ahmed S, Chaudhry MJ, Arshad M, Mahmood S, Ali A, Khan AA (2004) Diclofenac residues as the cause of vulture population decline in Pakistan. Nature 427:630–633
Galus M, Jeyaranjaan J, Smith E, Li H, Metcalfe C, Wilson JY (2013) Chronic effects of exposure to a pharmaceutical mixture and municipal wastewater in zebrafish. Aquat Toxicol 132–133:212–222
Cunningham VL, Binks SP, Olson MJ (2009) Human health risk assessment from the presence of human pharmaceuticals in the aquatic environment. Regul Toxicol Pharm 53:39–45
Mottaleb MA, Usenko S, O’Donnell JG, Ramirez AJ, Brooks BW, Chambliss CK (2009) Gas chromatography-mass spectrometry screening methods for select UV filters, synthetic musks, alkylphenols, an antimicrobial agent, and an insect repellent in fish. J Chromatogr A 1216:815–823
Ellis JB (2006) Pharmaceutical and personal care products (PPCPs) in urban receiving waters. Environ Pollut 144:184–189
Pereira AMPT, Silva LJG, Meisel LM, Lino CM, Pena A (2015) Environmental impact of pharmaceuticals from Portuguese wastewaters: geographical and seasonal occurrence, removal and risk assessment. Environ Res 136:108–119
Pavlović DM, Babić S, Horvat AJM, Kaštelan-Macan M (2007) Sample preparation in analysis of pharmaceuticals. TrAC Trend Anal Chem 26:1062–1075
Chen Y, Guo Z, Wang X, Qiu C (2008) Sample preparation. J Chromatogr A 1184:191–219
Ridgway K, Lalljie SP, Smith RM (2007) Sample preparation techniques for the determination of trace residues and contaminants in foods. J Chromatogr A 1153:36–53
Ramirez AJ, Mottaleb MA, Brooks BW, Chambliss CK (2007) Analysis of pharmaceuticals in fish using liquid chromatography-tandem mass spectrometry. Anal Chem 79:3155–3163
Martinez Bueno MJ, Boillot C, Fenet H, Chiron S, Casellas C, Gomez E (2013) Fast and easy extraction combined with high resolution-mass spectrometry for residue analysis of two anticonvulsants and their transformation products in marine mussels. J Chromatogr A 1305:27–34
Klosterhaus SL, Grace R, Hamilton MC, Yee D (2013) Method validation and reconnaissance of pharmaceuticals, personal care products, and alkylphenols in surface waters, sediments, and mussels in an urban estuary. Environ Int 54:92–99
Huerta B, Jakimska A, Gros M, Rodriguez-Mozaz S, Barcelo D (2013) Analysis of multi-class pharmaceuticals in fish tissues by ultra-high-performance liquid chromatography tandem mass spectrometry. J Chromatogr A 1288:63–72
Wang J, Gardinali PR (2012) Analysis of selected pharmaceuticals in fish and the fresh water bodies directly affected by reclaimed water using liquid chromatography-tandem mass spectrometry. Anal Bioanal Chem 404:2711–2720
Barker SA (2007) Matrix solid phase dispersion (MSPD). J Biochem Bioph Meth 70:151–162
Caldas SS, Bolzan CM, de Menezes EJ, Escarrone ALV, Martins CMG, Bianchini A, Primel EG (2013) A vortex-assisted MSPD method for the extraction of pesticide residues from fish liver and crab hepatopancreas with determination by GC-MS. Talanta 112:63–68
Sebastia N, Soler C, Soriano JM, Manes J (2010) Occurrence of aflatoxins in tigernuts and their beverages commercialized in Spain. J Agr Food Chem 58:2609–2612
Escarrone ALV, Caldas SS, Soares BM, Martins SE, Primel EG, Nery LEM (2014) A vortex-assisted MSPD method for triclosan extraction from fish tissues with determination by LC-MS/MS. Anal Meth 6:8306–8313
Barker SA, Long AR, Short CR (1989) Isolation of drug residues from tissues by solid phase dispersion. J Chromatogr A 475:353–361
Pensado L, Casais MC, Mejuto MC, Cela R (2005) Application of matrix solid-phase dispersion in the analysis of priority polycyclic aromatic hydrocarbons in fish samples. J Chromatogr A 1077:103–109
Sanchez-Brunete C, Miguel E, Tadeo JL (2008) Determination of organochlorine pesticides in sewage sludge by matrix solid-phase dispersion and gas chromatography-mass spectrometry. Talanta 74:1211–1217
Wang Z, Sun R, Wang Y, Li N, Lei L, Yang X, Yu A, Qui F, Zhang H (2014) Determination of phenolic acids and flavonoids in raw propolis by silica-supported ionic liquid-based matrix solid phase dispersion extraction high performance liquid chromatography-diode array detection. J Chromatogr B 969:205–212
Capriotti AL, Cavaliere C, Laganà A, Piovesana S, Samperi R (2013) Recent trends in matrix solid-phase dispersion. TrAC Trend Anal Chem 43:53–66
Garcia-Lopez M, Canosa P, Rodriguez I (2008) Trends and recent applications of matrix solid-phase dispersion. Anal Bioanal Chem 391:963–974
Duarte FA, Soares BM, Vieira AA, Pereira ER, Maciel JV, Caldas SS, Primel EG (2013) Assessment of modified matrix solid-phase dispersion as sample preparation for the determination of CH3Hg+ and Hg2+ in fish. Anal Chem 85:5015–5022
AOAC, Association of Official Analytical Chemists (2000) Official methods of analysis. AOAC International. Washington-DC
INMETRO (2010) Orientação sobre validação de métodos analíticos. DOQ-CGCRE-008, Brazil
SANCO (2013) Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed (Document n° SANCO/12571)
Pavlovic DM, Pinusic T, Perisa M, Babic S (2012) Optimization of matrix solid-phase dispersion for liquid chromatography tandem mass spectrometry analysis of 12 pharmaceuticals in sediments. J Chromatogr A 1258:1–15
Cerqueira MB, Caldas SS, Primel EG (2014) New sorbent in the dispersive solid phase extraction step of quick, easy, cheap, effective, rugged, and safe for the extraction of organic contaminants in drinking water treatment sludge. J Chromatogr A 1336:10–22
Kumar MNVR (2000) A review of chitin and chitosan applications. React Funct Polym 46:1–27
Kristenson E, Brinkman U, Ramos L (2006) Recent advances in matrix solid-phase dispersion. TrAC Trend Anal Chem 25:96–111
Al-Degs Y, Khraisheh MA, Tutunji MF (2001) Sorption of lead ions on diatomite and manganese oxides modified diatomite. Water Res 35:3724–3728
Tsai WT, Lai CW, Hsien KJ (2006) Characterization and adsorption properties of diatomaceous earth modified by hydrofluoric acid etching. J Colloid Interf Sci 297:749–754
Dotto GL, Vieira MLG, Pinto LAA (2012) Kinetics and mechanism of tartrazine adsorption onto chitin and chitosan. Ind Eng Chem Res 51:6862–6868
Hashemi M, Chasteen TG (2011) Hofmeister effect challenge. Anal Bioanal Chem 400:643–644
Shen ZL, Yuan D, Zhang H, Hu M, Zhu JH, Zhang HQ, Su QD (2011) Matrix solid phase dispersion-accelerated solvent extraction for determination of OCP residues in fish muscles. J Chin Chem Soc 58:494–502
Fan YB, Yin YM, Jiang WB, Chen YP, Yang JW, Wu J, Xie MX (2014) Simultaneous determination of ten steroid hormones in animal origin food by matrix solid-phase dispersion and liquid chromatography-electrospray tandem mass spectrometry. Food Chem 142:170–177
Tao Y, Zhu F, Chen D, Wei H, Pan Y, Wang X, Liu Z, Huang L, Wang Y, Yuan Z (2014) Evaluation of matrix solid-phase dispersion (MSPD) extraction for multi-fenicols determination in shrimp and fish by liquid chromatography-electrospray ionisation tandem mass spectrometry. Food Chem 150:500–506
Tsai DY, Chen CL, Ding DH (2014) Optimization of matrix solid-phase dispersion for the rapid determination of salicylate and benzophenone-type UV absorbing substances in marketed fish. Food Chem 154:211–216
Orlando EA, Simionato AV (2013) Extraction of tetracyclinic antibiotic residues from fish filet: comparison and optimization of different procedures using liquid chromatography with fluorescence detection. J Chromatogr A 1307:111–118
Lopes RP, Reyes RC, Romero-Gonzalez R, Vidal JL, Frenich AG (2012) Multiresidue determination of veterinary drugs in aquaculture fish samples by ultra high performance liquid chromatography coupled to tandem mass spectrometry. J Chromatogr B 895–896:39–47
Self RL, Wu WH (2012) Determination of eight biogenic amines in selected seafood products by MSPD extraction followed by UHPLC-Orbitrap MS. J Food Compos Anal 27:169–173
Acknowledgments
The authors acknowledge the financial support and fellowships granted by the Brazilian agencies CAPES, FINEP, and FURG. Part of this study was funded by CNPq/CAPES (process number 552318/2011-6), FAPERGS (process number 810-25.51/13-3), FAPERGS (process number 831-25.51/13-0), and CAPES/PNPD (process number 23038.028239/2009-69). E.G. Primel received a productivity research fellowship from the Brazilian Agency CNPq (DT 310517/2012-5).
Author information
Authors and Affiliations
Corresponding author
Electronic supplementary material
Below is the link to the electronic supplementary material.
ESM 1
(PDF 127 kb)
Rights and permissions
About this article
Cite this article
Hertzog, G.I., Soares, K.L., Caldas, S.S. et al. Study of vortex-assisted MSPD and LC-MS/MS using alternative solid supports for pharmaceutical extraction from marketed fish. Anal Bioanal Chem 407, 4793–4803 (2015). https://doi.org/10.1007/s00216-015-8685-3
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00216-015-8685-3