Rapid HPLC Method for Monitoring Relevant Residues of Pharmaceuticals Products in Environmental Samples


This work presents a multi-residue analytical method based on solid phase extraction (SPE) followed by high-performance liquid chromatographic (HPLC) with diode array (DAD) detection for the simultaneous determination of a group of pharmaceutical products that include ten antidepressants and three anticanceri- genic in environmental samples (water and soil). Baseline separation of the studied compounds was obtained on an ultrabase C18 (4.6 mm i.d. × 150 mm, 5 μm particle) column using acetonitrile:phosphate buffer pH 2.5 (35:65 v/v) as mobile phase with a flow rate of 1.5 mL/min. Different aspects including linearity, accuracy, precision and detection and quantification limits were examined in order to validate the proposed method. Detection limits between 1 and 50 ng/mL were obtained for all the target compounds. This method was ap- plied to the analysis of environmental samples as waters and soils of different precedence. Prior, the HPLC determination the samples were purified and enriched using SPE or liquid-liquid extraction (LLE) of the tar- get compounds.

Share and Cite:

Flores, J. , Salcedo, A. and Fernández, L. (2011) Rapid HPLC Method for Monitoring Relevant Residues of Pharmaceuticals Products in Environmental Samples. American Journal of Analytical Chemistry, 2, 18-26. doi: 10.4236/ajac.2011.21003.

Conflicts of Interest

The authors declare no conflicts of interest.


[1] T. Heberer, “Occurrence, Fate, and Removal of Pharmaceutical Residues in the Aquatic Environment: A Review of Recent Research Data,” Toxicology Letters, Vol. 131, 2002, pp. 5-17. doi:10.1016/S0378-4274(02)00041-3
[2] T. A. Ternes, “Occurence of Drugs in German Sewage Treatment Plant and Rivers,” Water Research, Vol. 32, 1998, pp. 3245-3260.
[3] W. P. Eckel, B. Ross and R. K. Isensee, “Pentobarbital Found in Ground Water,” Ground Water, Vol. 31, 1993, pp. 801-804. doi:10.1111/j.1745-6584.1993.tb00853.x
[4] J. V. Holm, K. Rügge, P. L. Bjerg and T. H. Christensen, “Occurrence and Distribution of Pharmaceutical Organic Compounds in the Groundwater Downgradient of a Landfill (Grindsted, Denmark),” Environmental Science & Technology, Vol. 29, 1995, pp. 1415-1420. doi:10.1021/es00005a039
[5] M. Ahel and I. Jelicic, “Phenazone Analgesics in Soil and Groundwater below a Municipal Solid Waste Landfill,” In: C. G. Daughton and T. Jones-Lepp, Eds., Pharmaceutical and Personal Care Products in the Environment: Scientific and Regulatory Issues. Symposium Series 791, American Chemical Society, Washington DC, 2001, pp. 100-115.
[6] K. Reddersen, T. Heberer and U. Dünnbier, “Identification and Significance of Phenazone Drugs and Their Metabolites in Ground and Drinking Water,” Chemosphere, Vol. 49, 2002, pp. 539-544. doi:10.1016/S0045-6535(02)00387-9
[7] K. Fent, A. A. Weston and D. Caminada, “Ecotoxicology of Human Pharmaceuticals,” Aquatic Toxicology, Vol. 76, 2006, pp. 122-159. doi:10.1016/j.aquatox.2005.09.009
[8] F. Sacher, F. T. Lange, H. J. Brauch and I. Blankenhorn, “Pharmaceuticlas in Groundwaters Analytical Methods and Results of a Monitoring Program in Baden-Württemberg Germany,” Journal of Chromatography A, Vol. 938, 2001, pp. 199-210. doi:10.1016/S0021-9673(01)01266-3
[9] G. L. Brun, M. Bernier, R. Losier, K. Doe, P. Jackman and H. B. Lee, “Pharmaceutically Active Compounds in Atlantic Canadian Sewage Treatment Plant Effluents and Receiving Waters, and Potential for Environmental Effects as Measured by Acute and Chronic Aquatic Toxicity,” Environmental Toxicology and Chemistry, Vol. 25, 2006, pp. 2163-2176. doi:10.1897/05-426R.1
[10] C. D. Metcalfe, X. S. Miao, B. G. Koening and J. Struger, “Distribution of Acidic and Neutral Drugs in Surface Waters Near Sewage Treatment Plants in the Lower Great Lakes, Canada,” Environmental Toxicology and Chemistry, Vol. 22, 2003, pp. 2881-2889. doi:10.1897/02-627
[11] T. A. Ternes, “Occurrence of Drugs in German Sewage Treatment Plants and Rivers,” Water Resources, Vol. 32, 1998, pp. 3245-3260. doi:10.1016/S0043-1354(98)00099-2
[12] T. A. Ternes, M. Bonerz and T. Schidt, “Determination of Neutral Pharmaceuticals in Wastewater and Rivers by Liquid Chromatography-Electrospray Tandem Mass Spectrometry,” Journal of Chromatography A, Vol. 938, 2001, pp. 175-185. doi:10.1016/S0021-9673(01)01205-5
[13] M. Farré, I. Ferrer, A. Ginebreda, M. Figueras, L. Oliv- ella, L. Tirapu, M. Vilanova and D. Barceló, “Determination of Drugs in Surface Water and Wastewater Samples by Liquid Chromatography-Mass Spectrometry: Methods and Preliminary Results Including Toxicity Studies with Vibrio Fischeri,” Journal of Chromatography A, Vol. 938, 2001, pp. 187-197. doi:10.1016/S0021-9673(01)01154-2
[14] I. Rodríguez, J. B. Quintana, J. Carpinteiro, A. M. Carro, R. A. Lorenzo and R. Cela, “Determination of Acidic Drugs in Sewage Water by Gás Chromatography-Mass Spectrometry as Tert-Butyldimethylsilyl Derivatives,” Journal of Chromatography A, Vol. 985, 2003 pp. 265-274. doi:10.1016/S0021-9673(02)01528-5
[15] I. Rodríguez, J. Carpinteiro, J. B. Quintana, A. M. Carro, R. A. Lorenzo and R. Cela, “Solid-Phase Microextraction with On-Fiber Derivation for the Analysis of Anti-Inflamatory Drugs in Water Samples,” Journal of Chromatography A, Vol. 1024, 2004, pp. 1-8. doi:10.1016/j.chroma.2003.10.049
[16] C. González-Barreiro, M. Lores, M. C. Cassis and R. Cela, “Simultaneous Determination of Neutral and Acidic Pharmaceuticals in Wastewater by High-Performance Liquid Chromatography-Post-Column Photochemically Induced Fluorimetry,” Journal of Chromatography A, Vol. 993, 2003, pp. 29-37. doi:10.1016/S0021-9673(03)00392-3
[17] W. Gebhardt and H. F. Schr?der, “Liquid Chromatography-(Tandem) Mass Spectrometry for the Follow-Up of the Elimination of Persistent Pharmaceuticals During Waste-Water Treatment Applying Biological Wastewater Treatment and Advanced Oxidation,” Journal of Chromatography A, Vol. 1160, 2007, pp. 34-43. doi:10.1016/j.chroma.2007.05.075
[18] C. Nebot, S. W. Gibb and K. G. Boyd, “Quantification of Human Pharmaceuticals in Water Samples by High Performance Liquid Chromatography-Tandem Mass Spectrometry,” Analytica Chimica Acta, Vol. 598, 2007, pp. 87-94. doi:10.1016/j.aca.2007.07.029
[19] S. L. MacLeod, P. Sudhir and C. S. Wong, “Stereoisomer Analysis of Wastewater-Derived Β-Blockers, Selective Serotonin Re-Uptake Inhibitors, and Salbutamol by High-Performance Liquid Chromatography-Tandem Mass Spectrometry,” Journal of Chromatography A, Vol. 1170, 2007, pp. 23-33. doi:10.1016/j.chroma.2007.09.010
[20] J. Radjenovic, M. Petrovic and D. Barceló, “Advanced Mass Spectrometric Method Applied to the Study off Ate and Renoval of Pharmaceuticals in Wastewater Treatment,” Trends in Analytical Chemistry, Vol. 26, 2007, pp. 1132-1144. doi:10.1016/j.trac.2007.10.002
[21] T. Vasskog, T. Anderssen, S. Pedersen-Bjergaard, R. Kallenborn and E. Jensen, “Occurrence of Selective Serotonin Reuptake Inhibitors in Sewage and Receiving Waters at Spitsbergen and in Norway,” Journal of Chromatography A, Vol. 1185, 2008, pp. 194-205. doi:10.1016/j.chroma.2008.01.063
[22] K. H. Langford and K. V. Thomas, “Determination of Pharmaceutical Compounds in Hospital Effluents and Their Contribution to Wastewater Treatment Works,” Environment International, Vol. 35, 2009, pp. 766-770. doi:10.1016/j.envint.2009.02.007
[23] M. J. Gómez, A. Agüera, M. Mezcua, J. Hurtado, F. Mo- cholí and A. R. Fernández-Alba, “Simultaneous Analysis of Neutral and Acidic Pharmaceuticals as Well as Related Compounds by Gas Chromatography-Tandem Mass Spectrometry in Wastewater,” Talanta, Vol. 73, 2007, pp. 314-320. doi:10.1016/j.talanta.2007.03.053
[24] L. Huber, “Applications of Diode-Array Experience,” Hewlett Packard, Waldbronn, 1989, Publication No. 12-5953-2330.

Copyright © 2024 by authors and Scientific Research Publishing Inc.

Creative Commons License

This work and the related PDF file are licensed under a Creative Commons Attribution 4.0 International License.