On-line solid-phase extraction of pharmaceutical compounds from wastewater treatment plant samples using restricted access media in column-switching liquid chromatography-tandem mass spectrometry

Júnior, César Augusto Marasco; Sartore, Douglas Morisue; Lamarca, Rafaela Silva; Silva, Bianca Ferreira da; Santos-Neto, Álvaro José; Gomes, Paulo Clairmont Feitosa de Lima

doi:10.1016/j.jchromb.2021.122896

Cited by 15 publications

(2 citation statements)

References 44 publications

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“…In our study, we aimed to establish an SPE method, based on online column-switching and this method in the field of online SPE enrichment [17][18][19] has gained significant prominence [20][21][22][23], which was more efficient, convenient, and faster than manual pre-processing samples. Besides, using a UV detector made the method more widely applicable and easier to standardize.…”

Section: Introductionmentioning

confidence: 99%

Trace determination of genotoxic impurity p‐toluene sulfonate alkyl esters in four active pharmaceutical ingredients by using on‐line column switching liquid chromatography

Jiang,

Zhao,

Sun

et al. 2024

Separation Science Plus

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Sulfonate esters, one of the genetic impurities, have gained significant attention in recent years due to their potential to cause genetic mutations and cancer. In this study, we reported a novel on‐line column‐switching liquid chromatography method for the quantitative analysis of three p‐toluene sulfonate alkyl esters in active pharmaceutical ingredients (APIs). The sensitivity was improved by large‐volume injection. A diluting modulation‐based sampling procedure was specifically devised to mitigate the impact of solvent effects and resolve the poor stability of isopropyl p‐toluene sulfonate alkyl ester. The established method was validated in terms of linearity, sensitivity, accuracy, stability, and robustness. The limit of quantitation level was determined to be 1 ng/mL (equivalent to 1 ppm relative to 1 mg/mL API samples). Besides, the method was applied for four APIs Tosuloxacin toluene sulfonate, Lapatinib toluene sulfonate, Nirapalib toluene sulfonate, and Capecitabine. The recoveries of all target analytes in the four‐drug substances were within 89%–110%. The expanded uncertainties of the measurements ranged from 6.8% to 8.4% at a coverage level of k = 2 and a confidence level of approximately 95%. The method described in this paper was compared with other published literature, demonstrating its simplicity and ease of standardization which could be further applied in the quality control and safety assessment of drug substances.

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Section: Introductionmentioning

confidence: 99%

Trace determination of genotoxic impurity p‐toluene sulfonate alkyl esters in four active pharmaceutical ingredients by using on‐line column switching liquid chromatography

Jiang,

Zhao,

Sun

et al. 2024

Separation Science Plus

View full text Add to dashboard Cite

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“…With the advances in instrumental analysis technology, the online-SPE technique enables automatic enrichment of target substances on the SPE column through automatic column switching, simplifying the pretreatment procedure, further improving detection efficiency, and reducing errors caused by manual operation [35,36]. The combination of online SPE and mass spectrometry has been successfully utilized to detect pharmaceutical and perfluorinated pollutants in water, with typical analysis times ranging from 15 to 30 min [37,38]. However, during LCMS analysis, background matter in water can affect the ionization efficiency in the ESI source of the mass spectrometer, resulting in significant enhancement or weakening of the target's mass spectral signal, known as the matrix effects [39].…”

Section: Introductionmentioning

confidence: 99%

An Online-SPE/SEC/LCMS Method for the Detection of N-Nitrosamine Disinfection Byproducts in Wastewater Plant Tailwater

Tang

Chen

et al. 2022

Water

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N-nitrosamines have recently attracted attention as a class of disinfection byproducts and are also a hot spot in environmental studies. Current N-nitrosamine analytical methods typically involve manual solid phase extraction (SPE) of samples followed by quantitative analysis using liquid chromatography-mass spectrometry (LCMS), which is time-consuming and may also fail to eliminate complex matrix effects. Size exclusion chromatography (SEC) is a technique that can separate compounds according to their molecular size. For the first time, this study developed an Online-SPE/SEC/LCMS quantitative analysis method to detect and analyze nine common N-nitrosamine disinfection byproducts in wastewater plant tailwater, including N-dimethylnitrosamine (NDMA) and N-nitrosodiethylamine (NDEA), etc. The samples of 1.0 mL can be directly injected after the simple 0.22 μm membrane filtration. This method reports the combination of SPE, SEC, and RP C18 columns to achieve several functions in a processing time of 20 min, including online enrichment, desalination, and matrix separation for the first time. The method provides good linearity (R2 > 0.999), recoveries ranging from 91.67% to 105.88%, relative standard deviation (RSD) lower than 4.17%, and the limits of detection (LOD) are 0.12–6.60 ng/L. This method alleviates tedious human labor and can effectively overcome the matrix effect (ME < 20%). This method allows for the accurate quantitative analysis of N-nitrosamines with high compatibility in wastewater plant tailwater, rivers, and lakes with a high background matrix. Interested researchers can also use this method as a reference in the online analysis of other specific pollutants after necessary optimization. It can also be utilized for non-targeted screening and targeted analysis of contaminants in water with a wide range of applications, giving valuable information for environmental monitoring.

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Flow analysis-solid phase extraction system and UHPLC-MS/MS analytical methodology for the determination of antiviral drugs in surface water

Mermer,

Jas,

Paluch

et al. 2024

Environ Sci Pollut Res

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An automated flow analysis-solid phase extraction (FA-SPE) system and methodology of ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) analysis were developed for the determination of selected antiviral drugs (acyclovir, amantadine, rimantadine, and oseltamivir) in water samples. The proposed FA-SPE approach enables the integration of various extraction stages and elimination of the sample evaporation step and offers individual customisation of SPE parameters, inter alia sample, and eluate flow rate and volume. Using the developed FA-SPE procedure, e.g. a 100-fold preconcentration of the target analytes in 1 h was achieved. A method for chromatographic analysis was also developed to determine the selected antiviral drugs in combination with the use of the FA-SPE system. The developed FA-SPE UHPLC-MS/MS method was validated including the determination of linearity of analytical graphs, limits of detection (5.5–99.9 pg mL−1) and quantification (18.3–329.8 pg mL−1), intra-day (1.8–8.3%) and inter-day (3.0–9.2%) precision, recovery (95.6–105.3%), and matrix effects (− 12.9 to 13.2%). The proposed method was successfully applied to analyse tap, drinking, and river water samples, revealing the presence of amantadine at a concentration of 40.1 pg mL−1 in one sample. The environmental impact of the developed FA-SPE sample preparation procedure was also assessed using the AGREEprep metric tool and compared with five other literature methods, achieving the most sustainable outcome. Graphical abstract

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On-line solid-phase extraction of pharmaceutical compounds from wastewater treatment plant samples using restricted access media in column-switching liquid chromatography-tandem mass spectrometry

Cited by 15 publications

References 44 publications

Trace determination of genotoxic impurity p‐toluene sulfonate alkyl esters in four active pharmaceutical ingredients by using on‐line column switching liquid chromatography

Trace determination of genotoxic impurity p‐toluene sulfonate alkyl esters in four active pharmaceutical ingredients by using on‐line column switching liquid chromatography

An Online-SPE/SEC/LCMS Method for the Detection of N-Nitrosamine Disinfection Byproducts in Wastewater Plant Tailwater

Flow analysis-solid phase extraction system and UHPLC-MS/MS analytical methodology for the determination of antiviral drugs in surface water

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