Disk solid-phase extraction of multi-class pharmaceutical residues in tap water and hospital wastewater, prior to ultra-performance liquid chromatographic-tandem mass spectrometry (UPLC-MS/MS) analyses

Kafeenah, Husam; Osman, Rozita; Bakar, Nor Kartini Abu

doi:10.1039/c8ra06885b

Cited by 26 publications

(15 citation statements)

References 46 publications

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“…However, this study did not compare the same type of sorbent in both formats. Kafeenah et al [103] did compare both formats using HLB sorbent. The method using disk SPE was better in terms of recovery, sensitivity, rapidness, and matrix effect, compared to the cartridge method.…”

Section: Spe Diskmentioning

confidence: 99%

Sample Preparation to Determine Pharmaceutical and Personal Care Products in an All-Water Matrix: Solid Phase Extraction

Sadutto

Picó

2020

Molecules

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Pharmaceuticals and personal care products (PPCPs) are abundantly used by people, and some of them are excreted unaltered or as metabolites through urine, with the sewage being the most important source to their release to the environment. These compounds are in almost all types of water (wastewater, surface water, groundwater, etc.) at concentrations ranging from ng/L to µg/L. The isolation and concentration of the PPCPs from water achieves the appropriate sensitivity. This step is mostly based on solid-phase extraction (SPE) but also includes other approaches (dispersive liquid-liquid microextraction (DLLME), buckypaper, SPE using multicartridges, etc.). In this review article, we aim to discuss the procedures employed to extract PPCPs from any type of water sample prior to their determination via an instrumental analytical technique. Furthermore, we put forward not only the merits of the different methods available but also a number of inconsistencies, divergences, weaknesses and disadvantages of the procedures found in literature, as well as the systems proposed to overcome them and to improve the methodology. Environmental applications of the developed techniques are also discussed. The pressing need for new analytical innovations, emerging trends and future prospects was also considered.

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Section: Spe Diskmentioning

confidence: 99%

Sample Preparation to Determine Pharmaceutical and Personal Care Products in an All-Water Matrix: Solid Phase Extraction

Sadutto

Picó

2020

Molecules

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“…According to the Eq. 2, the ion suppression (expressed as a percentage) was evaluated: the peak area in hospital wastewater extracts spiked with target compounds (AA) are first subtracted by the peak area of the compound in the non-spiked hospital wastewater extracts (AB), the values obtained are then compared with the peak area of the analyte in the standard solution water/methanol (50:50, v/v) spiked with the target compounds (AC) [33].…”

Section: Methods Validationmentioning

confidence: 99%

Determination of Pharmaceuticals Discharged in Wastewater from a Public Hospital Using LC-MS/MS Technique

et al. 2021

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Abstract. The presence of pharmaceuticals classified as emerging contaminants (EC) in surface water, groundwater, and drinking water generates uncertainty concerning the interactions that could be occurred with aquatic organisms and living beings. Thus, the monitoring of hospital wastewater is of great importance to identify the main classes of pharmaceuticals that could be discharged to the municipal sewage system and wastewater treatment plants (WWTPs). This work described the implementation and validation of a highly selective and sensitive analytical method using solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the detection and quantification of these emerging compounds. The solid-phase extraction (SPE) method was employed using Oasis HLB cartridges. For LC-MS/MS analysis, the chromatographic separation was conducted in a C-18 Kinetex column (Phenomenex), and detection was achieved in an AB SCIEX QTrap 3200 tandem mass spectrometer (MS/MS) in the multiple reaction monitoring (MRM) mode. The quantitative analysis was performed by using the internal standard (IS) method with isotopically labeled analogs. The implemented method presented good linearity within the concentration range of 0.1–400 µg L-1 showing correlation coefficients (R2) ranged from 0.991 to 0.999. The limits of detection (LODs) were from 0.02 to 0.59 µg L-1, while the limits of quantification (LOQs) ranged from 0.07 to 1.80 µg L-1. The analytical method was successfully applied to the analysis of wastewater samples discharged by a public hospital in San Nicolas de los Garza, Nuevo Leon, Mexico, in two sampling periods: May 2017 and March 2018. Resumen. La presencia de fármacos, clasificados como contaminantes emergentes, en agua superficial, subterránea y potable, genera incertidumbre sobre las interacciones que podrían ocurrir con organismos acuáticos y los seres vivos. Por lo tanto, el monitoreo del agua residual hospitalaria es de gran importancia para identificar los principales productos farmacéuticos que podrían descargarse al sistema de alcantarillado municipal y por lo tanto, estar presentes en el agua a tratar en las plantas de tratamiento de agua residual (PTAR). Este trabajo describe la implementación y validación de un método analítico altamente selectivo y sensible utilizando extracción en fase sólida (SPE) y cromatografía líquida acoplada a espectrometría de masas tándem (LC-MS/MS) para la detección y cuantificación de estos compuestos emergentes. Se empleó el método de extracción en fase sólida utilizando cartuchos Oasis HLB. Para el análisis LC-MS/MS, la separación cromatográfica se realizó en una columna Kinetex C-18 (Phenomenex), y la detección se realizó en un espectrómetro de masas en tándem AB SCIEX QTrap 3200 (MS/MS) en el modo de monitoreo de reacciones múltiples (MRM). El análisis cuantitativo se llevó a cabo utilizando el método de estándar interno (IS) con análogos marcados isotópicamente. El método presentó una buena linealidad dentro del rango de concentración de 0.1 a 400 µg L-1, con coeficientes de correlación (R2) que oscilaron entre 0.991 y 0.999. Los límites de detección (LOD) fueron de 0.02 a 0.59 µg L-1, mientras que los límites de cuantificación (LOQ) variaron de 0.07 a 1.80 µg L-1. El método analítico se aplicó con éxito al análisis de muestras de agua residual vertidas por un hospital público de San Nicolás de los Garza, Nuevo León, México, en dos períodos de muestreo: mayo de 2017 y marzo de 2018.

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“…Various instrumental methods have been applied for detection of DCF, including ultra-performance liquid chromatography (UPLC) coupled to high-resolution mass spectrometers [ 4 , 5 ]. However, these techniques are expensive and require extensive sample preparation [ 6 ].…”

Section: Introductionmentioning

confidence: 99%

Fluorescence polarization immunoassay for the determination of diclofenac in wastewater

et al. 2020

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Pharmacologically active compounds are often detected in wastewater and surface waters. The nonsteroidal anti-inflammatory drug diclofenac (DCF) was included in the European watch list of substances that requires its environmental monitoring in the member states. DCF may harmfully influence the ecosystem already at concentrations ≤ 1 μg L−1. The fast and easy quantification of DCF is becoming a subject of global importance. Fluorescence polarization immunoassay (FPIA) is a homogeneous mix-and-read method which does not require the immobilization of reagents. FPIA can be performed in one phase within 20–30 min, making it possible to analyse wastewater without any complicated pre-treatment. In this study, new tracer molecules with different structures, linking fluorophores to derivatives of the analyte, were synthesized, three homologous tracers based on DCF, two including a C6 spacer, and one heterologous tracer derived from 5-hydroxy-DCF. The tracer molecules were thoroughly assessed for performance. Regarding sensitivity of the FPIA, the lowest limit of detection reached was 2.0 μg L−1 with a working range up to 870 μg L−1. The method was validated for real wastewater samples against LC-MS/MS as reference method with good agreement of both methods.

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Disk solid-phase extraction of multi-class pharmaceutical residues in tap water and hospital wastewater, prior to ultra-performance liquid chromatographic-tandem mass spectrometry (UPLC-MS/MS) analyses

Abstract: A new sensitive analytical method was developed for pharmaceuticals with a very wide range of polarities, and log Kowranging from −0.5 to 5.12.

Cited by 26 publications

References 46 publications

Sample Preparation to Determine Pharmaceutical and Personal Care Products in an All-Water Matrix: Solid Phase Extraction

Sample Preparation to Determine Pharmaceutical and Personal Care Products in an All-Water Matrix: Solid Phase Extraction

Determination of Pharmaceuticals Discharged in Wastewater from a Public Hospital Using LC-MS/MS Technique

Fluorescence polarization immunoassay for the determination of diclofenac in wastewater

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