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Offline solid-phase extraction for preconcentration of pharmaceuticals and personal care products in environmental water and their simultaneous determination using the reversed phase high-performance liquid chromatography method

Abstract

The present study reports a precise and simple offline solid-phase extraction (SPE) coupled with reversed-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous determination of five representative and commonly present pharmaceuticals and personal care products (PPCPs), a new class of emerging pollutants in the aquatic environment. The target list of analytes including ciprofloxacin, acetaminophen, caffeine benzophenone and irgasan were separated by a simple HPLC method. The column used was a reversed-phase C18 column, and the mobile phase was 1 % acetic acid and methanol (20:80 v/v) under isocratic conditions, at a flow rate of 1 mL min−1. The analytes were separated and detected within 15 min using the photodiode array detector (PDA). The linearity of the calibration curves were obtained with correlation coefficients 0.98–0.99.The limit of detection (LOD), limit of quantification (LOQ), precision, accuracy and ruggedness demonstrated the reproducibility, specificity and sensitivity of the developed method. Prior to the analysis, the SPE was performed using a C18 cartridge to preconcentrate the targeted analytes from the environmental water samples. The developed method was applied to evaluate and fingerprint PPCPs in sewage collected from a residential engineering college campus, polluted water bodies such as Nag river and Pili river and the influent and effluent samples from a sewage treatment plant (STP) situated at Nagpur city, in the peak summer season. This method is useful for estimation of pollutants present in microquantities in the surface water bodies and treated sewage as compared to nanolevel pollutants detected by mass spectrometry (MS) detectors.

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References

  • Christian, G. D. (2004). Non-regulated water contaminants: emerging research. Environmental Impact Assessment Review, 24, 711.

    Article  Google Scholar 

  • Christian, G. D., & Thomas, A. T. (1999). Special report on “pharmaceuticals and personal care products in the environment: agents of subtle change? Environmental Health Perspectives, 107, 908–945.

    Google Scholar 

  • Emma, G. L., Juan, V. S., & Felix, H. (2010). Simultaneous determination of acidic, neutral and basic pharmaceuticals in urban wastewater by ultra high-pressure liquid chromatography-tandem mass spectrometry. Journal of Chromatography A, 1217, 622–632.

    Article  Google Scholar 

  • Emma, G. L., Juan, V. S., & Felix, H. (2011). Multi-class determination of around 50 pharmaceuticals, including 26 antibiotics, in environmental and wastewater samples by ultra-high performance liquid chromatography–tandem mass spectrometry. Journal of Chromatography A, 1218, 2264–2275.

    Article  Google Scholar 

  • Geetha, V. K., Harish, B. N., Srinivasan, R., & Yugendran, T. (2014). Plasmid-mediated quinolone resistance in typhoidal salmonellae: a preliminary report from South India. Indian Journal of Medical Microbiology, 32, 31–34.

    CAS  Article  Google Scholar 

  • Heberer, T. (2002). Occurrence, fate, and removal of pharmaceutical residues in the aquatic environment: a review of recent research data. Toxicology Letters, 131, 5–17.

    CAS  Article  Google Scholar 

  • Hillebrand, O., Nödler, K., Licha, T., Sauter, M., & Geyer, T. (2012). Caffeine as an indicator for the quantification of untreated wastewater in karst systems. Water Research, 46(2), 395–402.

    CAS  Article  Google Scholar 

  • Jimoh, O. T., Ojo, O. F., Lesile, F. P. (2013). A review of pharmaceuticals and endocrine disrupting compounds: sources, effects, removal, and detections. Water, Air, and Soil pollution. 224

  • Lloydr, S., Joseph, J.K., Joseph, L.G. (1997). Practical method development, second ed., New York.

  • Marta, P., Francesc, B., Rosa, M. M., & Eva, P. (2011). Analytical methods for personal-care products in environmental waters. Trends in Analytical Chemistry, 30, 750–760.

    Google Scholar 

  • Melanie, Lea H., Yelena, S., Paul, P, Allan, C., Andy, F., Edward, W. (2012). Pharmaceuticals and personal care products (PPCPs) in treated waste water discharges in to Charleston Harbor, South Carolina. Science of the Total Environment. 437.

  • Murat, K. (2001). LC method for analysis of paracetamol, caffeine and codeine phosphate in pharmaceutical preparations. Journal of Pharmaceuticals and Biomedical Analysis, 26, 857–864.

    Article  Google Scholar 

  • Prescott, L. F. (1980). Kinetics and metabolism of paracetamol and phenacetin. British Journal of Clinical Pharmacology, 10, 291–298.

    Article  Google Scholar 

  • Ranjit, S. (2013). HPLC method development and validation-an overview. Journal of Pharmaceutical, Education and Research, 4, 26–33.

    Google Scholar 

  • Raut, S. A., & Angus, R. A. (2010). Triclosan has endocrine-disrupting effects in male western mosquitofish, Gambusiaaffinis. Environmental Toxicology and Chemistry, 29, 1287–1291.

    CAS  Google Scholar 

  • Santiago, E., Daniele, M. B., Luiz, G. T. K., & Marcia, D. (2007). Ozonation and advanced oxidation technologies to remove endocrine disrupting chemicals (EDCs) and pharmaceuticals and personal care products (PPCPs) in water effluents. Journal of Hazardous Materials, 149, 631–642.

    Article  Google Scholar 

  • Santos, J. L., Aparicio, I., Alonso, E., & Callejon, M. (2005). Simultaneous determination of pharmaceutically active compounds in wastewater samples by solid phase extraction and high-performance liquid chromatography with diode array and fluorescence detectors. Analytica Chimica Acta, 550, 116–122.

    CAS  Article  Google Scholar 

  • Sara, C., Renzo, B., Davide, C., Roberto, F., & Ettore, Z. (2005). A multiresidue analytical method using solid-phase extraction and high-pressure liquid chromatography tandem mass spectrometry to measure pharmaceuticals of different therapeutic classes in urban wastewaters. Journal of Chromatography A, 1092, 206–215.

    Article  Google Scholar 

  • Schreiber, A. and Kern, R.O. (2010).Quantitation and identification of pharmaceuticals and personal care products (PPCP) in water samples, food and environmental.

  • Shahram, T., Paul, Y., Xiaoming, Z., Chunyan, H., Rajesh, S., Linda, S., and Taher, J. (2010). Occurrence and removal of PPCPs and EDCs in the Detroit River Watershed. Water practice and technology, 5.

  • Shanmugam, G., Ramasamy, K., Selvaraj, K. K., Sampath, S., & Ramaswam, B. R. (2014). Triclosan in fresh water fish Gibelion catla from the Kaveri river, India and its consumption risk assessment. Environmental Forensics, 15, 207–212.

    CAS  Article  Google Scholar 

  • Stephen, E. G., Chuan, W., & Yinfa, M. (2011). Determination of pharmaceutical and personal care products in wastewater by capillary electrophoresis with UV detection. Talanta, 84, 1163–1168.

    Article  Google Scholar 

  • Takatoril, S., Kitagawa, Y., Oda, H., Miwa, G., Nishikawa, J. I., Nishihara, T., Nakazawa, H., & Hori, S. (2003). Estrogenicity of metabolites of benzophenone derivatives examined by a yeast two-hybrid assay. Journal of Health Science, 49, 91–98.

    Article  Google Scholar 

  • Xiaoqin, W., Jeremy, L. C., & Jay, G. (2012). Multi-residue determination of pharmaceutical and personal care products in vegetables. Journal of Chromatography A, 1254, 78–86.

    Article  Google Scholar 

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Acknowledgments

The authors express thanks to Dr. Sachin A. Mandavgane of Chemical Engineering Department for providing the laboratory facilities for the sample preparation.

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Correspondence to Rita Dhodapkar or Anupama Kumar.

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G. Archana, Dhodapkar, R. & Kumar, A. Offline solid-phase extraction for preconcentration of pharmaceuticals and personal care products in environmental water and their simultaneous determination using the reversed phase high-performance liquid chromatography method. Environ Monit Assess 188, 512 (2016). https://doi.org/10.1007/s10661-016-5510-1

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  • DOI: https://doi.org/10.1007/s10661-016-5510-1

Keywords

  • Emerging pollutants
  • Pharmaceuticals and personal care products (PPCPs)
  • Ciprofloxacin
  • Acetaminophen
  • Caffeine
  • Benzophenone
  • Irgasan
  • Reverse-phase high-performance liquid chromatography (RP-HPLC)
  • Solid-phase extraction (SPE)
  • Wastewater analysis