Objective: Wastewater-based epidemiology is becoming a widespread technique with the ability to fill the gaps of conventional methods such as general population surveys, drug related deaths, seizure data. Studies on analytical techniques to identify consumption rates are more of a focus of interest than extraction methods even though sample extraction techniques have a noteworthy contribution to analysis results as well. The aim of this study was to compare two vacuum pressure manifold (negative and positive) systems in off-line solid-phase extraction (SPE) method in terms of extraction efficiency in wastewater for morphine (MOR), 6-monoacetylmorphine (6-MAM), amphetamine (AMP), methamphetamine (METH), 3,4-methylenedioxymethamphetamine (MDMA), benzoylecgonine (BE), cocaine (COC), 11-nor-Δ9-THC carboxylic acid (THC-COOH). Material and Methods: In this study, two different extraction set-ups were used to determine illicit drugs from wastewater and analysis were carried out by using Liquid Chromatography-Mass Spectrometry. Results: Correlation coefficients for all substances were found as r>0.999, LOD values were between 0.01-0.2 ng mL-1. Linear ranges of 6-MAM, METH, BE and COC were found between 0.2-100 ng mL-1, where the others' lowest calibration points were varying from 0.5 to 2 ng mL-1. Optimized SPE procedure was applied to both negative pressure manifold (NPM-SPE) and positive pressure manifold (PPM-SPE) by spiking tap water and wastewater samples separately. Conclusion: Efficiency differences were tested in terms of recovery, sample loading, time consumption, pressure control ability, and contamination sources. Overall recovery results revealed that there was no significant difference between PPM and NPM-SPE processes for both tap water and wastewater. Although set-ups have different superiorities to one another, it has been determined that the selection of the system should be made according to the type of targeted analytes and matrices.
Keywords: Sewage; forensic toxicology; solid phase extraction; waste water
Amaç: Atık su-tabanlı epidemiyolojik çalışmalar; anket araştırmaları, yasadışı madde kullanımına bağlı ölümler, ele geçirme verileri gibi geleneksel yöntemlere destek olan bir araçtır. Çekitleme tekniklerinin analiz sonuçlarına önemli katkı sağladığı bilinse de, tüketim oranlarını tayin etmek için kullanılan analitik teknikler çekitleme yöntemlerine göre daha çok ilgi odağı olmaktadır. Bu çalışmanın amacı, morfin (MOR), 6-monoasetilmorfin (6-MAM), amfetamin (AMP), metamfetamin (METH), 3,4-metilendioksimetamfetamin (MDMA), benzoilekgonin (BE), kokain (COC) ve 11-nor-Δ9-THC-karboksilik asit (THC-COOH) maddelerinin atık suda çekitleme verimi açısından, negatif ve pozitif basınçlı vakum sistemlerinin kullanıldığı manuel katı faz çekitleme (SPE) yöntemlerinin karşılaştırılmasıdır. Gereç ve Yöntemler: Bu çalışmada atık suda yasadışı madde tespiti için iki farklı çekitleme düzeneği kullanılmış ve tüm analizler Sıvı Kromatografi-Ardışık Kütle Spektrometresi sistemi kullanılarak yapılmıştır. Bulgular: Tüm maddeler için korelasyon katsayıları r>0,999, LOD değerleri 0,01-0,2 ng mL-1 arasında bulunmuştur. 6-MAM, METH, BE ve COC'nin doğrusal aralıkları 0,2-100 ng mL-1 arasında bulunurken, diğer kalibrasyon noktalarının en düşükleri ise 0,5-2 ng mL-1 arasında değişmektedir. Belirlenen SPE prosedürü, musluk suyu ve atık su numuneleri kirletilerek hem negatif basınç (NPM-SPE) hem de pozitif basınç (PPM-SPE) kullanılan düzeneklerde uygulanmıştır. Sonuç: Düzenekler arasındaki verim farklılıkları, geri kazanım, numune yükleme, zaman tüketimi, basınç kontrol yeteneği ve kontaminasyon kaynakları bakımından değerlendirilmiştir. Tüm geri-kazanım sonuçlarına bakıldığında, hem musluk suyu hem de atık su için, PPM ve NPM-SPE arasında anlamlı bir fark olmadığı bulunmuştur. Her ne kadar basınç düzeneklerinin birbirine göre üstünlükleri olsa da, sistemin seçiminin, hedeflenen analiz ve matrikslerin türüne göre yapılması gerektiği düşünülmektedir.
Anahtar Kelimeler: Lağım; sıvı atık; adli toksikoloji; solid faz çıkartımı; atık su
- Löve ASC, Baz-Lomba JA, Reid MJ, Kankaanpää A, Gunnar T, Dam M, et al. Analysis of stimulant drugs in the wastewater of five Nordic capitals. Sci Total Environ. 2018;627:1039-47. [Crossref] [PubMed]
- Mastroianni N, López-García E, Postigo C, Barceló D, López de Alda M. Five-year monitoring of 19 illicit and legal substances of abuse at the inlet of a wastewater treatment plant in Barcelona (NE Spain) and estimation of drug consumption patterns and trends. Sci Total Environ. 2017;609:916-26. [Crossref] [PubMed]
- Rico M, Andrés-Costa MJ, Picó Y. Estimating population size in wastewater-based epidemiology. Valencia metropolitan area as a case study. J Hazard Mater. 2017;323(Pt A):156-65.
- European Monitoring Centre for Drugs and Drug Addiction (EMCDDA). Country Drug Report 2017. ISBN: 978-92-9497-030-5. Turkey, Lisbon: 2017. p.18.
- European Monitoring Centre for Drugs and Drug Addiction (EMCDDA). Country Drug Report 2018. Turkey, Lisbon: 2018. [Crossref]
- European Monitoring Centre for Drugs and Drug Addiction (EMCDDA). Key Indicators; 2015. (accessed date: 12.07.2018). [Link]
- European Monitoring Centre for Drugs and Drug Addiction (EMCDDA). Insights Series No 9. Assessing illicit drugs in wastewater Potential and limitations of a new monitoring approach. Luxemburg: 2008. ISBN 978-929168-317-8.
- European Monitoring Centre for Drugs and Drug Addiction (EMCDDA). Assessing illicit drugs in wastewater: advances in wastewaterbased drug epidemiology. Insights 22. Publications Office of the European Union, Luxembourg: 2016. p.77. doi: 10.2810/017397.
- González-Mariño I, Quintana JB, Rodríguez I, González-Díez M, Cela R. Screening and selective quantification of illicit drugs in wastewater by mixed-mode solid-phase extraction and quadrupole-time-of-flight liquid chromatography-mass spectrometry. Anal Chem. 2012;84(3):1708-17. [Crossref] [PubMed]
- Hogenboom AC, van Leerdam JA, de Voogt P. Accurate mass screening and identification of emerging contaminants in environmental samples by liquid chromatography-hybrid linear ion trap orbitrap mass spectrometry. J Chromatogr A. 2009;1216(3):510-9. [Crossref] [PubMed]
- Wilson JF, Smith BL, Toseland PA, Watson ID, Williams J, Thomson AH, et al. A survey of extraction techniques for drugs of abuse in urine. Forensic Sci Int. 2001;119(1):23-7. [Crossref]
- Drummer OH. Chromatographic screening techniques in systematic toxicological analysis. J Chromatogr B Biomed Sci Appl. 1999;733(1-2):27-45. [Crossref]
- van Wel JH, Kinyua J, van Nuijs AL, Salvatore S, Bramness JG, Covaci A, et al. A comparison between wastewater-based drug data and an illicit drug use survey in a selected community. Int J Drug Policy. 2016;34:20-6. [Crossref] [PubMed]
- van Nuijs AL, Castiglioni S, Tarcomnicu I, Postigo C, Lopez de Alda M, Neels H, et al. Illicit drug consumption estimations derived from wastewater analysis: a critical review. Sci Total Environ. 2011;409(19):3564-77. [Cross - ref] [PubMed]
- Bijlsma L, Botero-Coy AM, Rincón RJ, Peñuela GA, Hernández F. Estimation of illicit drug use in the main cities of Colombia by means of urban wastewater analysis. Sci Total Environ. 2016;565:984-93. [Crossref] [PubMed]
- Bijlsma L, Beltrán E, Boix C, Sancho JV, Hernández F. Improvements in analytical methodology for the determination of frequently consumed illicit drugs in urban wastewater. Anal Bioanal Chem. 2014;406(17): 4261-72. [Crossref] [PubMed]
- Irvine RJ, Kostakis C, Felgate PD, Jaehne EJ, Chen C, White JM. Population drug use in Australia: a wastewater analysis. Forensic Sci Int. 2011;210(1-3):69-73. [Crossref] [PubMed]
- Tscharke BJ, Chen C, Gerber JP, White JM. Temporal trends in drug use in Adelaide, South Australia by wastewater analysis. Sci Total Environ. 2016;565:384-91. [Crossref] [PubMed]
- Löve ASC, Baz-Lomba JA, Reid MJ, Kankaanpää A, Gunnar T, Dam M, et al. Analysis of stimulant drugs in the wastewater of five Nordic capitals. Sci Total Environ. 2018;627:1039-47. [Crossref] [PubMed]
- Baker DR, Kasprzyk-Hordern B. Critical evaluation of methodology commonly used in sample collection, storage and preparation for the analysis of pharmaceuticals and illicit drugs in surface water and wastewater by solid phase extraction and liquid chromatography-mass spectrometry. J Chromatogr A. 2011;1218(44):8036-59. [Crossref] [PubMed]
- Vazquez-Roig P, Blasco C, Picó Y. Advances in the analysis of legal and illegal drugs in the aquatic environment. Trends Anal Chem. 2013;50:65-77. [Crossref]
- Castiglioni S, Thomas KV, Kasprzyk-Hordern B, Vandam L, Griffiths P. Testing wastewater to detect illicit drugs: state of the art, potential and research needs. Sci Total Environ. 2014;487:613-20. [Crossref] [PubMed]
- van Nuijs AL, Tarcomnicu I, Bervoets L, Blust R, Jorens PG, Neels H, et al. Analysis of drugs of abuse in wastewater by hydrophilic interaction liquid chromatography-tandem mass spectrometry. Anal Bioanal Chem. 2009; 395(3):819-28. [Crossref] [PubMed]
- Postigo C, de Alda MJ, Barceló D. Fully automated determination in the low nanogram per liter level of different classes of drugs of abuse in sewage water by on-line solid-phase extraction-liquid chromatography-electrospraytandem mass spectrometry. Anal Chem. 2008;80(9):3123-34. [Crossref] [PubMed]
- Postigo C, de Alda ML, Barceló D. Evaluation of drugs of abuse use and trends in a prison through wastewater analysis. Environ Int. 2011;37(1):49-55. [Crossref] [PubMed]
- Kim EM, Lee JS, Choi SK, Lim MA, Chung HS. Analysis of ketamine and norketamine in urine by automatic solid-phase extraction (SPE) and positive ion chemical ionizationgas chromatography-mass spectrometry (PCIGC-MS). Forensic Sci Int. 2008;174(2-3): 197-202. [Crossref] [PubMed]
- Baker DR, Kasprzyk-Hordern B. Multiresidue analysis of drugs of abuse in wastewater and surface water by solid-phase extraction and liquid chromatography-positive electrospray ionisation tandem mass spectrometry. J Chromatogr A. 2011; 1218(12):1620-31. [Crossref] [PubMed]
- Castiglioni S, Bijlsma L, Covaci A, Emke E, Hernández F, Reid M, et al. Evaluation of uncertainties associated with the determination of community drug use through the measurement of sewage drug biomarkers. Environ Sci Technol. 2013;47(3):145-60. [Crossref] [PubMed]
- Jacox A, Wetzel J, Cheng SY, Concheiro M. Quantitative analysis of opioids and cannabinoids in wastewater samples. Forensic Sci Res. 2017;2(1):18-25. [Crossref] [PubMed] [PMC]
- Causanilles A, Baz-Lomba JA, Burgard DA, Emke E, González-Mariño I, Krizman-Matasic I, et al. Improving wastewater-based epidemiology to estimate cannabis use: focus on the initial aspects of the analytical procedure. Anal Chim Acta. 2017;988:27-33. [Crossref] [PubMed]
- González-Mariño I, Quintana JB, Rodríguez I, Rodil R, González-Peñas J, Cela R. Comparison of molecularly imprinted, mixed-mode and hydrophilic balance sorbents performance in the solid-phase extraction of amphetamine drugs from wastewater samples for liquid chromatography-tandem mass spectrometry determination. J Chromatogr A. 2009; 1216(48):8435-41. [Crossref] [PubMed]
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