Analysis of Personal Care Products in Sediments and Soils

  • Sarah Montesdeoca-Esponda
  • Tanausú Vega-Morales
  • Zoraida Sosa-Ferrera
  • José Juan Santana-RodríguezEmail author
Part of the The Handbook of Environmental Chemistry book series (HEC, volume 36)


Sample extraction and preparation methods are described for the most relevant groups of personal care products (PCPs) (disinfectants, fragrances, preservatives, UV filters and stabilisers) in solid samples from aquatic environments. The extraction methodologies have been separated into two groups, conventional and novel procedures, to compare the improvements and advantages implemented in recent years to produce more efficient and simple methods. The difficulties related to the treatment of solid samples and to complex matrices are discussed in depth. The analytical methods employed after the extraction procedures, all of which are based on mass spectrometry detection, are also covered. Finally, an overview of the measured concentration of these families of PCPs in the environment is provided, which can be useful in the establishment of future trends.


Extraction techniques Gas chromatography Liquid chromatography Personal care products Solid samples 



1H benzotriazole














4-Methylbenzylidene camphor






Celestolide or 4-acetyl-1,1-dimethyl-6-tert-butylindan


Phantolide or 6-acetyl-1,1,2,3,3,5-hexamethylindan


Tonalide or 7-acetyl-1,1,3,4,4,6–hexamethyl-1,2,3,4-tetrahydronaphthalene




Traseolide or 5-acetyl-1,1,2,6-tetramethyl-3-isopropylindan
















2-Hydroxy-phenylmethyl ester benzoic acid






Cashmeran or 1,2,3,5,6,7-Hexahydro-1,1,2,3,3-pentamethyl-4H-inden-4-one


Ethylhexyl methoxycinnamate


Ethylhexyl salicylate

etocrylene; EC









Galaxolid or 1,3,4,6,7,8-Hexahydro-4,6,6,7,8,8-hexamethylcyclopenta(g)-2-benzopyran






Isoamyl methoxycinnamate






Musk ketone or 4-tert-butyl-3,5-dinitro-2,6-dimethylacetophenone




Musk xylene or 1-tert-butyl-3,5-di-methyl-2,4,6-trinitrobenzene



Octocrylene; OC


Octyl Salicylate; OS



Ethylhexyldimethyl p-aminobenzoate




2-(5-t-butyl-2-hydroxyphenyl) benzotriazole






2-(4,6-Diphenyl-1,3,5-triazine-2-yl)-5-[(hexyl) oxy]-phenol










2-(2′-Hydroxy-3′,5′-di-tert-amylphenyl) benzotriazole


2-(2H-benzotriazol-2-yl)-4-(1,1,3,3-tetramethylbutyl) phenol








  1. 1.
    Ternes TA, Joss A, Siegrist H (2004) Scrutinizing pharmaceuticals and personal care products in wastewater treatment. Environ Sci Technol 38:392–399CrossRefGoogle Scholar
  2. 2.
    Wille K, De Brabander HF, De Wulf E, Van Caeter P, Janssen CR, Vanhaecke L (2012) Coupled chromatographic and mass-spectrometric techniques for the analysis of emerging pollutantsin the aquatic environment. Trends Anal Chem 35:87–108CrossRefGoogle Scholar
  3. 3.
    Sosa-Ferrera Z, Mahugo-Santana C, Santana-Rodríguez JJ (2013) Analytical methodologies for the determination of endocrine disrupting compounds in biological and environmental samples. Biomed Res Int. doi: 10.1155/2013/674838 Google Scholar
  4. 4.
    Kronimus A, Schwarzbauer J, Dsikowitzky L, Heim S, Littke R (2004) Anthropogenic organic contaminants in sediments of the Lippe river, Germany. Water Res 38:3473–3484CrossRefGoogle Scholar
  5. 5.
    Zhao JL, Ying GG, Liu YS, Chen F, Yang JF, Wang L (2010) Occurrence and risks of triclosan and triclocarban in the Pearl River system. J Hazard Mater 179:215–222CrossRefGoogle Scholar
  6. 6.
    Chen ZF, Ying GG, Lai HJ, Chen F, Su HC, Liu HS, Peng FQ, Zhao JL (2012) Determination of biocides in different environmental matrices by use of ultra-high-performance liquid chromatography–tandem mass spectrometry. Anal Bioanal Chem 404:3175–3188CrossRefGoogle Scholar
  7. 7.
    Peck AM (2006) Analytical methods for the determination of persistent ingredients of personal care products in environmental matrices. Anal Bioanal Chem 386:907–939CrossRefGoogle Scholar
  8. 8.
    Zeng X, Mai B, Sheng G, Lou X, Shao W, An T, Fu J (2008) Distribution of polycyclic musks in surface sediments from the Pearl River Delta and Macao coastal region, South China. Environ Toxicol Chem 27:18–23CrossRefGoogle Scholar
  9. 9.
    Núñez L, Tadeo JL, García-Valcárcel AI, Turiel E (2008) Determination of parabens in environmental solid samples by ultrasonic-assisted extraction and liquid chromatography with triple quadrupole mass spectrometry. J Chromatogr A 1214:178–182CrossRefGoogle Scholar
  10. 10.
    Núñez L, Turiel E, Martin-Esteban A, Tadeo JL (2010) Molecularly imprinted polymer for the extraction of parabens from environmental solid samples prior to their determination by high performance liquid chromatography–ultraviolet detection. Talanta 80:1782–1788CrossRefGoogle Scholar
  11. 11.
    Liao C, Lee S, Moon HB, Yamashita N, Kannan K (2013) Parabens in sediment and sewage sludge from the United States, Japan, and Korea: Spatial distribution and temporal trends. Environ Sci Technol 47:10895–10902CrossRefGoogle Scholar
  12. 12.
    Jeon HK, Chung Y, Ryu JC (2006) Simultaneous determination of benzophenone-type UV filters in water and soil by gas chromatography–mass spectrometry. J Chromatogr A 1131:192–202CrossRefGoogle Scholar
  13. 13.
    Sánchez-Brunete C, Miguel E, Albero B, Tadeo JL (2011) Analysis of salicylate and benzophenone-type UV filters in soils and sediments by simultaneous extraction cleanup and gas chromatography–mass spectrometry. J Chromatogr A 1218:4291–4298CrossRefGoogle Scholar
  14. 14.
    Kameda Y, Kimura K, Miyazaki M (2011) Occurrence and profiles of organic sun-blocking agents in surface waters and sediments in Japanese rivers and lakes. Environ Pollut 159:1570–1576CrossRefGoogle Scholar
  15. 15.
    Zhang Z, Ren N, Li Y, Kunisue T, Gao D, Kannan K (2011) Determination of benzotriazole and benzophenone UV Filters in sediment and sewage sludge. Environ Sci Technol 45:3909–3916CrossRefGoogle Scholar
  16. 16.
    Nakata H, Murata S, Filatreau J (2009) Occurrence and concentrations of benzotriazole UV stabilizers in marine organisms and sediments from the Ariake Sea, Japan. Environ Sci Technol 43:6920–6926CrossRefGoogle Scholar
  17. 17.
    Guo JH, Li HX, Cao HL, Li Y, Wang XZ, Xu XB (2009) Determination of triclosan, triclocarban and methyl-triclosan in aqueous samples by dispersive liquid-liquid microextraction combined with rapid liquid chromatography. J Chromatogr A 1216:3038–3043CrossRefGoogle Scholar
  18. 18.
    Brausch JM, Rand GM (2011) A review of personal care products in the aquatic environment: Environmental concentrations and toxicity. Chemosphere 82:1518–1532CrossRefGoogle Scholar
  19. 19.
    Schramm KW, Kaune A, Beck B, Thumm W, Behechti A, Kettrup A, Nickolova P (1996) Acute toxicities of five nitromusk compounds in Daphnia, algae and photoluminescent bacteria. Water Res 30:2247–2250CrossRefGoogle Scholar
  20. 20.
    Balk F, Ford RA (1999) Environmental risk assessment for the polycyclic musks, AHTN and HHCB II. Effect assessment and risk characterization. Toxicol Lett 111:81–94CrossRefGoogle Scholar
  21. 21.
    Buchberger WW (2011) Current approaches to trace analysis of pharmaceuticals and personal care products in the environment. J Chromatogr A 1218:603–618CrossRefGoogle Scholar
  22. 22.
    Bester K (2009) Analysis of musk fragrances in environmental samples. J Chromatogr A 1216:470–480CrossRefGoogle Scholar
  23. 23.
    Pietrogrande MC, Basaglia G (2007) GC–MS analytical methods for the determination of personal-care products in water matrices. Trends Anal Chem 26:1086–1094CrossRefGoogle Scholar
  24. 24.
    Díaz-Cruz MS, Barceló D (2009) Chemical analysis and ecotoxicological effects of organic UV-absorbing compounds in aquatic ecosystems. Trends Anal Chem 28:708–717CrossRefGoogle Scholar
  25. 25.
    Montesdeoca-Esponda S, Vega-Morales T, Sosa Ferrera Z, Santana Rodríguez JJ (2013) Extraction and determination methodologies for benzotriazole UV stabilizers in personal-care products in environmental and biological samples. Trends Anal Chem 51:23–32CrossRefGoogle Scholar
  26. 26.
    Camel V (2001) Recent extraction techniques for solid matrices-supercritical fluid extraction, pressurized fluid extraction and microwave-assisted extraction: their potential and pitfalls. Analyst 126:1182–1193CrossRefGoogle Scholar
  27. 27.
    Zuloaga O, Navarro P, Bizkarguenaga E, Iparraguirre A, Vallejo A, Olivares M, Prieto A (2012) Overview of extraction, clean-up and detection techniques for the determination of organic pollutants in sewage sludge: a review. Anal Chim Acta 736:7–29CrossRefGoogle Scholar
  28. 28.
    Montesdeoca-Esponda S, Sosa-Ferrera Z, Santana-Rodríguez JJ (2013) Microwave assisted extraction combined with on-line solid phase extraction followed by ultra-high-performance liquid chromatography with tandem mass spectrometry determination of benzotriazole UV stabilisers in marine sediments and sewage sludges. J Sep Sci 36:781–787CrossRefGoogle Scholar
  29. 29.
    Peck AM, Hornbuckleb KC (2004) Synthetic musk fragrances in lake Michigan. Environ Sci Technol 38:367–372CrossRefGoogle Scholar
  30. 30.
    Schwarzbauer J, Littke R, Weigelt V (2000) Identification of specific organic contaminants for estimating the contribution of the Elbe river to the pollution of the German Bight. Organ Geochem 31:1713–1731CrossRefGoogle Scholar
  31. 31.
    Tadeo JL, Sánchez-Brunete C, Albero B, García-Valcárcel AI, Pérez RA (2012) Analysis of emerging organic contaminants in environmental solid samples. Cent Eur J Chem 10:480–520CrossRefGoogle Scholar
  32. 32.
    Agüera A, Fernández-Alba AR, Piedra L, Mézcua M, Gómez MJ (2003) Evaluation of triclosan and biphenylol in marine sediments and urban wastewaters by pressurized liquid extraction and solid phase extraction followed by gas chromatography mass spectrometry and liquid chromatography mass spectrometry. Anal Chim Acta 480:193–205CrossRefGoogle Scholar
  33. 33.
    Morales S, Canosa P, Rodríguez I, Rubí E, Cela R (2005) Microwave assisted extraction followed by gas chromatography with tandem mass spectrometry for the determination of triclosan and two related chlorophenols in sludge and sediments. J Chromatogr A 1082:128–135CrossRefGoogle Scholar
  34. 34.
    Morales-Muñoz S, Luque-García JL, Ramos MJ, Martínez-Bueno MJ, Luque de Castro MD (2005) Sequential automated focused microwave-assisted soxhlet extraction of compounds with different polarity from marine sediments prior to gas chromatography mass spectrometry detection. Chromatographia 62:69–74CrossRefGoogle Scholar
  35. 35.
    Morales-Muñoz S, Luque-García JL, Ramos MJ, Fernández-Alba A, Luque de Castro MD (2005) Sequential superheated liquid extraction of pesticides, pharmaceutical and personal care products with different polarity from marine sediments followed by gas chromatography mass spectrometry detection. Anal Chim Acta 552:50–59CrossRefGoogle Scholar
  36. 36.
    Rice SL, Mitra S (2007) Microwave-assisted solvent extraction of solid matrices and subsequent detection of pharmaceuticals and personal care products (PPCPs) using gas chromatography–mass spectrometry. Anal Chim Acta 589:125–132CrossRefGoogle Scholar
  37. 37.
    Burkhardt MR, ReVello RC, Smith SG, Zaugg SD (2005) Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for industrial and anthropogenic waste-indicator compounds in sediment. Anal Chim Acta 534:89–100CrossRefGoogle Scholar
  38. 38.
    Casas-Ferreira AM, Möder M, Fernández-Laespada ME (2011) Stir bar sorptive extraction of parabens, triclosan and methyl triclosan from soil, sediment and sludge with in situ derivatization and determination by gas chromatography–mass spectrometry. J Chromatogr A 1218:3837–3844CrossRefGoogle Scholar
  39. 39.
    González-Mariño I, Rodríguez I, Quintana JB, Cela R (2010) Matrix solid-phase dispersion followed by gas chromatography-mass spectrometry for the determination of triclosan and methyl triclosan in sludge and sediments. Anal Bioanal Chem 398:2289–2297CrossRefGoogle Scholar
  40. 40.
    Wu SF, Ding WH (2010) Fast determination of synthetic polycyclic musks in sewage sludge and sediments by microwave-assisted headspace solid-phase microextraction and gas chromatography-mass spectrometry. J Chrom A 1217:2776–2781CrossRefGoogle Scholar
  41. 41.
    Delgado B, Pino V, Anderson JL, Ayala JH, Afonso AM, González V (2012) An in-situ extraction–preconcentration method using ionic liquid-based surfactants for the determination of organic contaminants contained in marine sediments. Talanta 99:972–983CrossRefGoogle Scholar
  42. 42.
    Rodil R, Moeder M (2008) Development of a simultaneous pressurised-liquid extraction and clean-up procedure for the determination of UV filters in sediments. Anal Chim Acta 612:152–159CrossRefGoogle Scholar
  43. 43.
    Carpinteiro I, Abuín B, Ramil M, Rodríguez I, Cela R (2012) Matrix solid-phase dispersion followed by gas chromatography tandem mass spectrometry for the determination of benzotriazole UV absorbers in sediments. Anal Bioanal Chem 402:519–527CrossRefGoogle Scholar
  44. 44.
    Carabias-Martínez R, Rodríguez-Gonzalo E, Revilla-Ruiz P, Hernández-Méndez J (2005) Pressurized liquid extraction in the analysis of food and biological samples. J Chromatogr A 1089:1–17CrossRefGoogle Scholar
  45. 45.
    Dabrowski L, Giergielewicz-Mozajska H, Biziuk M, Gaca J, Namiésnik J (2002) Some aspects of the analysis of environmen- tal pollutants in sediments using pressurized liquid extraction and gas chromatography-mass spectrometry. J Chromatogr A 957:59–67CrossRefGoogle Scholar
  46. 46.
    Chienthavorn O, Poonsukcharoen T, Pathrakorn T (2011) Pressurized liquid and superheated water extraction of active constituents from zingiber cassumunar roxb. rhizome. Sep Sci Technol 46:616–624CrossRefGoogle Scholar
  47. 47.
    Pérez-Serradilla JA, Japón-Luján R, Luque de Castro MD (2008) Static–dynamic sequential superheated liquid extraction of phenols and fatty acids from alperujo. Anal Bioanal Chem 392:1241–1248CrossRefGoogle Scholar
  48. 48.
    Pedrouzo M, Borrull F, Marcé RM, Pocurull E (2011) Analytical methods for personal-care products in environmental waters. Trends Anal Chem 30:749–760CrossRefGoogle Scholar
  49. 49.
    Wick A, Fink G, Ternes TA (2010) Comparison of electrospray ionization and atmospheric pressure chemical ionization for multi-residue analysis of biocides, UV-filters and benzothiazoles in aqueous matrices and activated sludge by liquid chromatography-tandem mass spectrometry. J Chromatogr A 1217:2088–2103CrossRefGoogle Scholar
  50. 50.
    Blair BD, Crago JP, Hedman CJ, Klaper RD (2013) Pharmaceuticals and personal care products found in the Great Lakes above concentrations of environmental concern. Chemosphere 93:2116–2123CrossRefGoogle Scholar
  51. 51.
    Angelov T, Vlasenko A, Tashkov W (2008) HPLC determination of pKa of parabens and investigation on their lipophilicity parameters. J Liquid Chromatogr Rel Technol 31:188–197CrossRefGoogle Scholar
  52. 52.
    Montesdeoca-Esponda S, Sosa-Ferrera Z, Santana-Rodríguez JJ (2012) On-line solid-phase extraction coupled to ultra-performance liquid chromatography with tandem mass spectrometry detection for the determination of benzotriazole UV stabilizers in coastal marine and wastewater samples. Anal Bioanal Chem 403:867–876CrossRefGoogle Scholar
  53. 53.
    Montesdeoca-Esponda S, Toro-Moreno D, Sosa-Ferrera Z, Santana-Rodríguez JJ (2013) Development of a sensitive determination method for benzotriazole UV stabilizers in enviromental water samples with stir bar sorption extraction and liquid desorption prior to ultra-high performance liquid chromatography with tándem mass spectrometry. J Sep Sci 36:2168–2175CrossRefGoogle Scholar
  54. 54.
    Ruan T, Liu R, Fu Q, Wang T, Wang Y, Song S, Wang P, Teng M, Jiang G (2012) Concentrations and composition profiles of benzotriazole UV stabilizers in municipal sewage sludge in China. Environ Sci Technol 46:2071–2079CrossRefGoogle Scholar
  55. 55.
    Blair BD, Crago JP, Hedman CJ, Treguer RJF, Magruder C, Royer LS, Klaper RD (2013) Evaluation of a model for the removal of pharmaceuticals, personal care products, and hormones from wastewater. Sci Total Environ 444:515–521CrossRefGoogle Scholar
  56. 56.
    USEPA (2007) Method 1694: pharmaceuticals and personal care products in water, soil, sediment, and biosolids by HPLC/MS/MS. United Stated Environmental Protection Agency, Washington DCGoogle Scholar
  57. 57.
    Annesley TM (2003) Ion suppression in mass spectrometry. Clin Chem 49:1041–1044CrossRefGoogle Scholar
  58. 58.
    Kim JW, Isobe T, Ramaswamy BR, Chang KH, Amano A, Miller TM, Siringan FP, Tanabe S (2011) Contamination and bioaccumulation of benzotriazole ultraviolet stabilizers in fish from Manila Bay, the Philippines using an ultrafast liquid chromatography-tandem mass spectrometry. Chemosphere 85:751–758CrossRefGoogle Scholar
  59. 59.
    Reemtsma T (2003) LC-MS and strategies for trace-level analysis of polar organic pollutants. J Chromatogr A 1000:477–501CrossRefGoogle Scholar
  60. 60.
    Creaser CS, Stygall JW (1993) Particle beam liquid chromatography-mass spectrometry: instrumentation and applications. A review Analyst 118:1467–1480CrossRefGoogle Scholar
  61. 61.
    Glish GL, Vachet RW (2003) The basics of mass spectrometry in the twenty-first century. Nat Rev 2:140–149Google Scholar

Copyright information

© Springer International Publishing Switzerland 2014

Authors and Affiliations

  • Sarah Montesdeoca-Esponda
    • 1
  • Tanausú Vega-Morales
    • 1
  • Zoraida Sosa-Ferrera
    • 1
  • José Juan Santana-Rodríguez
    • 1
    Email author
  1. 1.Departamento de QuímicaUniversidad de Las Palmas de Gran CanariaLas Palmas de Gran CanariaSpain

Personalised recommendations