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
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