Abstract
The development of analytical methods capable of determining micropollutants is essential for quality control of drinking water. Benzodiazepines, a class of pharmaceuticals with anxiolytic properties, have received increasing attention as micropollutants. The purpose of this study was to develop an analytical method for determination of three benzodiazepine drugs (bromazepam, clonazepam and diazepam) in surface water. For the extraction of the matrix analytes, SPE cartridges (C18, 500 mg/3 mL) were used. The method was validated according to the quality criteria of the USEPA 8000D Validation Guide. The developed and validated method showed recovery values between 57 and 100%, RSD < 20% and R2 > 0.9949. LD ranged between 2.70 and 5.00 ng L−1 for bromazepam and clonazepam respectively whereas LQ was 0.01 μg L−1 for all analytes. The matrix affected the signal intensity of clonazepam thus evidencing the matrix effect by analysis statistic (F test).
Similar content being viewed by others
References
Andreu V, Gimeno-García E, Pascual JA et al (2016) Presence of pharmaceuticals and heavy metals in the waters of a Mediterranean coastal wetland: potential interactions and the influence of the environment. Sci Total Environ 540:278–286. https://doi.org/10.1016/j.scitotenv.2015.08.007
Arbeláez P, Borrull F, Pocurull E, Marcé RM (2015) Determination of high-intensity sweeteners in river water and wastewater by solid-phase extraction and liquid chromatography-tandem mass spectrometry. J Chromatogr A 1393:106–114. https://doi.org/10.1016/j.chroma.2015.03.035
Aymerich I, Acuña V, Barceló D et al (2016) Attenuation of pharmaceuticals and their transformation products in a wastewater treatment plant and its receiving river ecosystem. Water Res 100:126–136. https://doi.org/10.1016/j.watres.2016.04.022
Bonfiglio R, King RC, Olah TV, Merkle V (1999) The effects of sample preparation methods on the variability of the electrospray ionization response for model drug compounds. Rapid Commun Mass Spectrom 13(12):1175-1185. https://doi.org/10.1002/(SICI)1097-0231(19990630)13:12<1175::AID-RCM639>3.0.CO;2-0
Brieudes V, Lardy-Fontan S, Lalere B et al (2016) Validation and uncertainties evaluation of an isotope dilution-SPE-LC-MS/MS for the quantification of drug residues in surface waters. Talanta 146:138–147. https://doi.org/10.1016/j.talanta.2015.06.073
Caldas SS, Rombaldi C, de Oliveira Arias JL et al (2016) Multi-residue method for determination of 58 pesticides, pharmaceuticals and personal care products in water using solvent demulsification dispersive liquid–liquid microextraction combined with liquid chromatography-tandem mass spectrometry. Talanta 146:676–688. https://doi.org/10.1016/j.talanta.2015.06.047
Cetesb (2011) Guia Nacional de Coleta e Preservação de Amostras - Água, Sedimento. Comunidades Aquáticas e Efluentes Líquidos, Cia Ambient do Estado São Paulo
Cunha DL, de Araujo FG, Marques M (2017) Psychoactive drugs: occurrence in aquatic environment, analytical methods, and ecotoxicity—a review. Environ Sci Pollut Res 24:24076–24091. https://doi.org/10.1007/s11356-017-0170-4
Dai G, Huang J, Chen W et al (2014) Major pharmaceuticals and personal care products (PPCPs) in wastewater treatment plant and receiving water in Beijing, China, and associated ecological risks. Bull Environ Contam Toxicol 92:655–661. https://doi.org/10.1007/s00128-014-1247-0
de Almeida CAA, Oliveira MS, Mallmann CA, Martins AF (2015) Determination of the psychoactive drugs carbamazepine and diazepam in hospital effluent and identification of their metabolites. Environ Sci Pollut Res 22:17192–17201. https://doi.org/10.1007/s11356-015-4948-y
Ferreira AP (2014) Environmental investigation of psychiatric pharmaceuticals: Guandu River, Rio De Janeiro State, Southeast Brazil. J Chem Heal Risks 4:25–32
García-Galán MJ, Petrovic M, Rodríguez-Mozaz S, Barceló D (2016) Multiresidue trace analysis of pharmaceuticals, their human metabolites and transformation products by fully automated on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry. Talanta 158:330–341. https://doi.org/10.1016/j.talanta.2016.05.061
Gros M, Petrovic M (2009) Tracing pharmaceutical residues of different therapeutic classes in environmental waters by using liquid chromatography/quadrupole-linear ion trap mass spectrometry and automated library searching. Anal Chem 81:898–912
Gros M, Rodríguez-mozaz S, Barceló D (2012) Fast and comprehensive multi-residue analysis of a broad range of human and veterinary pharmaceuticals and some of their metabolites in surface and treated waters by ultra-high-performance liquid chromatography coupled to quadrupole-linear ion trap tandem. J Chromatogr A 1248:104–121. https://doi.org/10.1016/j.chroma.2012.05.084
INCB (2015) International Narcotics Contol Board Psychotropic Substances—Statistics for 2013. INCB, New York
Luo Y, Guo W, Ngo HH et al (2014) A review on the occurrence of micropollutants in the aquatic environment and their fate and removal during wastewater treatment. Sci Total Environ 473–474:619–641. https://doi.org/10.1016/j.scitotenv.2013.12.065
Mann O, Pock E, Wruss K et al (2016) Development and validation of a fully automated online-SPE–ESI–LC–MS/MS multi-residue method for the determination of different classes of pesticides in drinking, ground and surface water. Int J Environ Anal Chem 96:353–372. https://doi.org/10.1080/03067319.2016.1160381
Matsuo H, Sakamoto H, Arizono K, Shinohara R (2011) Behavior of pharmaceuticals in waste water treatment plant in Japan. Bull Environ Contam Toxicol 87:31–35. https://doi.org/10.1007/s00128-011-0299-7
Postigo C, De Alda MJL, Barceló D (2008) Fully automated determination in the low nanogram per liter level of different classes of drugs of abuse in sewage water by on-line chromatography—electrospray-tandem mass spectrometry. Anal Chem 80:3123–3134. https://doi.org/10.1021/ac702060j
Silveira MAK, Caldas SS, Guilherme JR et al (2013) Quantification of pharmaceuticals and personal care product residues in surface and drinking water samples by SPE and LC-ESI-MS/MS. J Braz Chem Soc 24:1385–1395. https://doi.org/10.5935/0103-5053.20130176
Stipaničev D, Dragun Z, Repec S et al (2017) Broad spectrum screening of 463 organic contaminants in rivers in Macedonia. Ecotoxicol Environ Saf 135:48–59. https://doi.org/10.1016/j.ecoenv.2016.09.004
Tran NH, Hu J, Ong SL (2013) Talanta Simultaneous determination of PPCPs, EDCs, and arti fi cial sweeteners in environmental water samples using a single-step SPE coupled with HPLC–MS/MS and isotope dilution. Talanta 113:82–92. https://doi.org/10.1016/j.talanta.2013.03.072
USEPA (2014) SW 846 test method 8000D: determinative chromatographic separations.
Valls-Cantenys C, Scheurer M, Iglesias M et al (2016) A sensitive multi-residue method for the determination of 35 micropollutants including pharmaceuticals, iodinated contrast media and pesticides in water. Anal Bioanal Chem 408:6189–6200. https://doi.org/10.1007/s00216-016-9731-5
Acknowledgements
The authors acknowledge the financial support provided by the Coordination and Improvement of Higher Level or Education Personnel (CAPES) to the first author (Process 1589040/2016); by the National Council for Scientific and Technological Development (CNPq) (Process 308.335/2017-1) to the third author and; by the Carlos Chagas Filho Research Support Foundation (FAPERJ) (Processes E-26/202.894/2018 and E-26/202.793/2015) to the third and fourth authors, respectively.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
de Araujo, F.G., Bauerfeldt, G.F., Marques, M. et al. Development and Validation of an Analytical Method for the Detection and Quantification of Bromazepam, Clonazepam and Diazepam by UPLC-MS/MS in Surface Water. Bull Environ Contam Toxicol 103, 362–366 (2019). https://doi.org/10.1007/s00128-019-02631-z
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00128-019-02631-z