Determination of 89 drugs and other micropollutants in unfiltered wastewater and freshwater by LC-MS/MS: an alternative sample preparation approach

Abstract

A liquid chromatography-triple quadrupole-tandem mass spectrometry (LC-qQq-MS/MS) method was developed for simultaneous determination of 89 legal neuropsychiatric pharmaceuticals and illicit drugs (both parent compounds and metabolites) and other micropollutants in unfiltered wastewater and freshwater. The target chemicals fall under the classes of amphetamine-type stimulants, cocaine compounds, opiates and opioids, benzodiazepines, lysergic compounds, antipsychotics, anesthetics, antiepileptics, antidepressants, sympathomimetics, cannabinoids, blood thinners, antihistamines, β-blockers, caffeine derivatives, nicotine derivatives, z-drugs, new designer drugs, and Alzheimer medications. The sample preparation procedure was designed for unfiltered wastewater and freshwater without the need to separate the particulate matter (if any) from the aqueous phase prior to extraction. Samples were pre-concentrated by rotary evaporation in the presence of a solvent. Method precision (absolute values; N = 6 replicate analyses at the fortification level of 50 ng, k = 6 days) for 87 out of 89 target analytes ranged from 2.8 to 34% (RSD %). The limits of detection ranged from 0.11 to 202 ng L, and the matrix effects ranged from +16 to -84%. A total of 10 samples, 8 wastewater, 1 drinking water, and 1 lake water, were collected from New York State, USA, and were analyzed for the target compounds to demonstrate the applicability of the developed method. This is the first study to report the analysis of multiple classes of pharmaceuticals, illicit drugs, and other micropollutants in unfiltered wastewater. Graphical abstract Analysis of 89 micropollutants in unfiltered wastewater by LC-MS/MS.

A Survey of the Presence of Pharmaceutical Residues in Wastewaters. Evaluation of Their Removal using Conventional and Natural Treatment Procedures

“…In this sense, some compounds like caffeine and nicotine and their respective metabolites paraxanthine and cotinine, and some broadly used drugs like naproxen or acetaminophen are usually detected at higher concentrations (in the range of µg•L −1 ) than other pharmaceuticals. Other common pharmaceuticals like diclofenac, erythromycin or carbamazepine are usually in the range of ng•L −1 as previous research has indicated [10][11][12]. However, many studies evaluate the occurrence of pharmaceuticals during a short period of time; few studies examine these compounds in the long term to evaluate seasonal fluctuations and determine patterns from the presence of these compounds.…”

Fragmentation pathways of protonated coumarin by ESI‐QE‐Orbitrap‐MS/MS coupled with DFT calculations

“…In recent years, mass spectrometry has become an important tool in many fields such as pharmaceutics and life science, because of the characteristic of rapidity, sensitivity, and feasibility . As a soft ionization MS, electrospray ionization coupled with quadrupole extractive orbitrap MS (ESI‐QE‐Orbitrap‐MS/MS) could provide the accurate mass data for precursor and fragment ions.…”

Bazı Antidepresan ve Antiepileptik İlaçların İnsan Kanında Eş Zamanlı Analizi için LC-MS/MS Yöntemi Geliştirilmesi

“…İnsan vücudu dışında yapılan çalışmalar da ise şehirlerin atık sularında bulunan antidepresanların LC-MS/MS ile eş zamanlı tayini yapılmış ve 38 psikoaktif ilacın (benzodiazepinler, antidepresanlar ve istismar ilaçları dahil) ortalama ve maksimum konsantrasyon seviyelerinin literatürde daha önce rapor edilen seviyelerin üzerinde çıktığı bulunmuştur. 2017 yılında Sıvı Kromatografi-Üçlü Dört Kutuplu Tandem Kütle Spektrometresi (LC-MS/MS) yöntemi ile 89 yasal nöropsikiyatrik ilaç ve yasadışı uyuşturucunun (hem ana bileşikler hem de metabolitler) filtre edilmemiş atık su ve tatlı suda eş zamanlı belirlenmesi için metot geliştirilmiştir [12][13][14].…”