Determination of 27 pharmaceuticals and personal care products (PPCPs) in water: The benefit of isotope dilution

  • Xueqi Fan
  • Jie Gao
  • Wenchao Li
  • Jun HuangEmail author
  • Gang Yu
Research Article


Pharmaceuticals and personal care products (PPCPs) are a unique group of emerging and nonpersistent contaminants. In this study, 27 PPCPs in various water samples were extracted by solid phase extraction (SPE), and determined by isotope dilution method using liquid chromatography coupled to tandem triple quadruple mass spectrometer (LC-MS/MS). A total of 27 isotopically labeled standards (ILSs) were applied to correct the concentration of PPCPs in spiked ultrapure water, drinking water, river, effluent and influent sewage. The corrected recoveries were 73%–122% with the relative standard deviation (RSD) < 16%, except for acetaminophen. The matrix effect for all kinds of water samples was < 22% and the method quantitation limits (MQLs) were 0.45–8.6 ng/L. The developed method was successfully applied on environmental water samples. The SPE extracts of spiked ultrapure water, drinking water, river and wastewater effluent were stored for 70 days, and the ILSs-corrected recoveries of 27 PPCPs were obtained to evaluate the correction ability of ILSs in the presence of variety interferences. The recoveries of 27 PPCPs over 70 days were within the scope of 72%–140% with the recovery variation < 37% in all cases. The isotope dilution method seems to be of benefit when the extract has to be stored for long time before the instrument analysis.


Pharmaceuticals and personal care products (PPCPs) Isotopically labeled standard (ILSs) Water Solid-phase extraction (SPE) LC-MS/MS 



This work was supported by the Major Science and Technology Program for Water Pollution Control and Treatment in China (Nos. 2017ZX07202-001 and 2017ZX07202-004).

Supplementary material

11783_2019_1187_MOESM1_ESM.pdf (28 kb)
Supporting materials


  1. Ali A M, Rønning H T, Sydnes L K, Alarif W M, Kallenborn R, Al-Lihaibi S S (2018). Detection of PPCPs in marine organisms from contaminated coastal waters of the Saudi Red Sea. Science of the Total Environment, 621: 654–662CrossRefGoogle Scholar
  2. Aristizabal-Ciro C, Botero-Coy A M, López F J, Peñuela G A (2017). Monitoring pharmaceuticals and personal care products in reservoir water used for drinking water supply. Environmental Science and Pollution Research International, 24(8): 7335–7347CrossRefGoogle Scholar
  3. Biel-Maeso M, Corada-Fernández C, Lara-Martín P A (2019). Removal of personal care products (PCPs) in wastewater and sludge treatment and their occurrence in receiving soils. Water Research, 150: 129–139CrossRefGoogle Scholar
  4. Caban M, Lis E, Kumirska J, Stepnowski P (2015). Determination of pharmaceutical residues in drinking water in Poland using a new SPE-GC-MS(SIM) method based on Speedisk extraction disks and DIMETRIS derivatization. Science of the Total Environment, 538: 402–411CrossRefGoogle Scholar
  5. Cai M Q, Wang R, Feng L, Zhang L Q (2015). Determination of selected pharmaceuticals in tap water and drinking water treatment plant by high-performance liquid chromatography-triple quadrupole mass spectrometer in Beijing, China. Environmental Science and Pollution Research International, 22(3): 1854–1867CrossRefGoogle Scholar
  6. Chen F, Gong Z, Kelly B C (2015). Rapid analysis of pharmaceuticals and personal care products in fish plasma micro-aliquots using liquid chromatography tandem mass spectrometry. Journal of Chromatography. A, 1383: 104–111CrossRefGoogle Scholar
  7. Díaz A, Peña-Alvarez A (2017). A simple method for the simultaneous determination of pharmaceuticals and personal care products in river sediment by ultrasound-assisted extraction followed by solid-phase microextraction coupled with gas chromatography-mass spectrometry. Journal of Chromatographic Science, 55(9): 946–953CrossRefGoogle Scholar
  8. Du B, Perez-Hurtado P, Brooks B W, Chambliss C K (2012). Evaluation of an isotope dilution liquid chromatography tandem mass spectrometry method for pharmaceuticals in fish. Journal of Chromatography. A, 1253: 177–183CrossRefGoogle Scholar
  9. Ebele A J, Abdallah M A, Harrad S (2017). Pharmaceuticals and personal care products (PPCPs) in the freshwater aquatic environment. Emerging Contaminants, 3(1): 1–16CrossRefGoogle Scholar
  10. Fan X, Zhao S, Hu J (2019). Dissipation behavior and dietary risk assessment of lambda-cyhalothrin, thiamethoxam and its metabolite clothianidin in apple after open field application. Regulatory Toxicology and Pharmacology, 101: 135–141CrossRefGoogle Scholar
  11. Gómez M J, Martínez Bueno M J, Lacorte S, Fernández-Alba A R, Agüera A (2007). Pilot survey monitoring pharmaceuticals and related compounds in a sewage treatment plant located on the Mediterranean coast. Chemosphere, 66(6): 993–1002CrossRefGoogle Scholar
  12. Hao C, Zhao X, Yang P (2007). GC-MS and HPLC-MS analysis of bioactive pharmaceuticals and personal care products in environmental matrices. Trends in Analytical Chemistry, 26(6): 569–580CrossRefGoogle Scholar
  13. Huang H, Wu J, Ye J, Ye T, Deng J, Liang Y, Liu W (2018). Occurrence, removal, and environmental risks of pharmaceuticals in wastewater treatment plants in south China. Frontiers of Environmental Science & Engineering 12(6): 7CrossRefGoogle Scholar
  14. Jiang X, Qu Y, Liu L, He Y, Li W, Huang J, Yang H, Yu G (2019). PPCPs in a drinking water treatment plant in the Yangtze River Delta of China: Occurrence, removal and risk assessment. Frontiers of Environmental Science & Engineering, 13(2): 27CrossRefGoogle Scholar
  15. Jiménez J J, Sánchez M I, Pardo R, Muñoz B E (2017). Degradation of indomethacin in river water under stress and non-stress laboratory conditions: degradation products, long-term evolution and adsorption to sediment. Journal of environmental sciences-China, 51: 13–20CrossRefGoogle Scholar
  16. Lin T, Yu S, Chen W (2016). Occurrence, removal and risk assessment of pharmaceutical and personal care products (PPCPs) in an advanced drinking water treatment plant (ADWTP) around Taihu Lake in China. Chemosphere, 152: 1–9CrossRefGoogle Scholar
  17. Löffler D, Römbke J, Meller M, Ternes T A (2005). Environmental fate of pharmaceuticals in water/sediment systems. Environmental Science & Technology, 39(14): 5209–5218CrossRefGoogle Scholar
  18. Monteiro S C, Boxall A B (2009). Factors affecting the degradation of pharmaceuticals in agricultural soils. Environmental Toxicology and Chemistry, 28(12): 2546–2554CrossRefGoogle Scholar
  19. Oliveira T S, Murphy M, Mendola N, Wong V, Carlson D, Waring L (2015). Characterization of pharmaceuticals and personal care products in hospital effluent and waste water influent/effluent by direct-injection LC-MS-MS. Science of the Total Environment, 518–519: 459–478CrossRefGoogle Scholar
  20. Papageorgiou M, Kosma C, Lambropoulou D (2016). Seasonal occurrence, removal, mass loading and environmental risk assessment of 55 pharmaceuticals and personal care products in a municipal wastewater treatment plant in Central Greece. Science of the Total Environment, 543(Pt A): 547–569CrossRefGoogle Scholar
  21. Petrie B, McAdam E J, Scrimshaw M D, Lester J N, Cartmell E (2013). Fate of drugs during wastewater treatment. Trends in Analytical Chemistry, 49(49): 145–159CrossRefGoogle Scholar
  22. Primel E G, Caldas S S, Escarrone A L (2012). Multi-residue analytical methods for the determination of pesticides and PPCPs in water by LC-MS/MS: A review. Central European Journal of Chemistry, 10(3): 876–899Google Scholar
  23. Rivera-Jaimes J A, Postigo C, Melgoza-Alemán R M, Aceña J, Barceló D, López de Alda M (2018). Study of pharmaceuticals in surface and wastewater from Cuernavaca, Morelos, Mexico: Occurrence and environmental risk assessment. Science of the Total Environment, 613–614: 1263–1274CrossRefGoogle Scholar
  24. Sui Q, Huang J, Deng S, Yu G, Fan Q (2010). Occurrence and removal of pharmaceuticals, caffeine and DEET in wastewater treatment plants of Beijing, China. Water Research, 44(2): 417–426CrossRefGoogle Scholar
  25. Tanoue R, Nomiyama K, Nakamura H, Hayashi T, Kim J W, Isobe T, Shinohara R, Tanabe S (2014). Simultaneous determination of polar pharmaceuticals and personal care products in biological organs and tissues. Journal of Chromatography. A, 1355: 193–205CrossRefGoogle Scholar
  26. Tran N H, Hu J, Ong S L (2013). Simultaneous determination of PPCPs, EDCs, and artificial sweeteners in environmental water samples using a single-step SPE coupled with HPLC-MS/MS and isotope dilution. Talanta, 113(17): 82–92CrossRefGoogle Scholar
  27. Tran N H, Li J, Hu J, Ong S L (2014). Occurrence and suitability of pharmaceuticals and personal care products as molecular markers for raw wastewater contamination in surface water and groundwater. Environmental Science and Pollution Research International, 21(6): 4727–4740CrossRefGoogle Scholar
  28. USEPA (2007). Method 1694: Pharmaceuticals and Personal Care Products in Water, Soil, Sediment, and Biosolids by HPLC/MS/MS. Washington, DC: US Environmental Protection AgencyGoogle Scholar
  29. Wang J, Wang S (2016). Removal of pharmaceuticals and personal care products (PPCPs) from wastewater: A review. Journal of Environmental Management, 182: 620–640CrossRefGoogle Scholar
  30. Yang Y, Yong S O, Kim K H, Kwon E E, Tsang Y F (2017). Occurrences and removal of pharmaceuticals and personal care products (PPCPs) in drinking water and water/sewage treatment plants: A review. Science of the Total Environment, 596–597: 303–320CrossRefGoogle Scholar
  31. Zhang Y, Guo W, Yue Z, Lin L, Zhao F, Chen P, Wu W, Zhu H, Yang B, Kuang Y, Wang J (2017). Rapid determination of 54 pharmaceutical and personal care products in fish samples using microwave-assisted extraction-Hollow fiber-Liquid/solid phase microextraction. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1051: 41–53CrossRefGoogle Scholar

Copyright information

© Higher Education Press and Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  • Xueqi Fan
    • 1
  • Jie Gao
    • 1
  • Wenchao Li
    • 2
  • Jun Huang
    • 1
    Email author
  • Gang Yu
    • 1
  1. 1.State Key Joint Laboratory of Environment Simulation and Pollution Control (SKJLESPC), Beijing Key Laboratory for Emerging Organic Contaminants Control (BKLEOC), School of EnvironmentTsinghua UniversityBeijingChina
  2. 2.CSD IDEA (Beijing) Environment Test & Analysis Co., Ltd.BeijingChina

Personalised recommendations