Multi-residue analysis of pharmaceuticals in aqueous environmental samples by online solid-phase extraction–ultra-high-performance liquid chromatography-tandem mass spectrometry: Optimisation and matrix effects reduction by quick, easy, cheap, effective, rugged and safe extraction

Bourdat-Deschamps, Marjolaine; Leang, Sokha; Bernet, Nicolas; Daudin, Jean‐Jacques; Nélieu, Sylvie

doi:10.1016/j.chroma.2014.05.006

Cited by 84 publications

(48 citation statements)

References 43 publications

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“…Stock solutions of each standard compound and each deuterated labelled compound, as well as the multi-compound working solutions, were prepared and stored as described by Bourdat-Deschamps et al [25]. McIlvaine and citrate buffers were prepared by mixing 0.1 M citric acid and 0.2 M disodium phosphate and 0.1 M citric acid and 0.1 M sodium citrate, respectively, at different proportions to obtain pH ranging from 2.5 to 9.…”

Section: Chemicals and Reagentsmentioning

confidence: 99%

Factors influencing the extraction of pharmaceuticals from sewage sludge and soil: an experimental design approach

et al. 2016

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Pharmaceuticals can enter the environment when organic waste products are recycled on agricultural soils. The extraction of pharmaceuticals is a challenging step in their analysis. The very different extraction conditions proposed in the literature make the choice of the right method for multi-residue analysis difficult. This study aimed at evaluating, with experimental design methodology, the influence of the nature, pH and composition of the extraction medium on the extraction recovery of 14 pharmaceuticals, including 8 antibiotics, from soil and sewage sludge. Preliminary experimental designs showed that acetonitrile and citrate-phosphate buffer were the best extractants. Then, a response surface design demonstrated that many cross-product and squared terms had significant effects, explaining the shapes of the response surfaces. It also allowed optimising the pharmaceutical recoveries in soil and sludge. The optimal conditions were interpreted considering the ionisation states of the compounds, their solubility in the extraction medium and their interactions with the solid matrix. To perform the analysis, a compromise was made for each matrix. After a QuEChERS purification, the samples were analysed by online SPE-UHPLC-MS-MS. Both methods were simple and economical. They were validated with the accuracy profile methodology for soil and sludge and characterised for another type of soil, digested sludge and composted sludge. Trueness globally ranged between 80 and 120 % recovery, and inter- and intra-day precisions were globally below 20 % relative standard deviation. Various pharmaceuticals were present in environmental samples, with concentration levels ranging from a few micrograms per kilogramme up to thousands of micrograms per kilogramme. Graphical abstract Influence of the extraction medium on the extraction recovery of 14 pharmaceuticals. Influence of the ionisation state, the solubility and the interactions of pharmaceuticals with solid matrix. Analysis of different soils and organic waste products.

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Section: Chemicals and Reagentsmentioning

confidence: 99%

Factors influencing the extraction of pharmaceuticals from sewage sludge and soil: an experimental design approach

et al. 2016

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“…At the same time for the quantification of the analyte from marketed formulations and in bulk a proper sample preparation procedure is often required when the excepients in formulations (suspensions, lotions, creams) interferes with the analyte 36 . In such cases sample pretreatment is often necessary [27][28][29][30][31][32][33][34][35][36] . Thus possible chromatographic interferences and clogging or detoriation of the column can be avoided.…”

Section: Methodology: 21 Sample Preparationmentioning

confidence: 99%

“…A number of chromatographic techniques have been developed in last two decades for the quantification of newer fluoroquinolones 14-22 from a variety of sample matrices. The introduction of chromatographic techniques has revolutionized the process of detection, separation and quantification of the parent components and the respective metabolites with higher selectivity, sensitivity, precession and accuracy form a variety of sample matrices including biological and environmental matrices [22][23][24][25][26][27][28][29][30][31][32][33][34][35] . Moreover these chromatographic techniques can be derived from available techniques with slight modification or can be developed on the basis of knowledge gathered through experience and physical properties of the analyte under consideration.…”

Section: Available Analytical Techniques For the Quantification Of Qumentioning

confidence: 99%

Untitled

2016

IJPSR

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ABSTRACT:Fluoroquinolones are the most commonly prescribed synthetic antibacterial agents having improved pharmacokinetic properties and broad spectrum of activity. Due to their broad clinical activity they are the most promising drug for antibacterial chemotherapy. The current study focused on the application of similar chromatographic system for the analysis of a number of fluoroquinolones from bulk, pharmaceutical formulations and biological matrices. We have also summarized how a single chromatographic system can be used for the quantification of a number of fluoroquinoloes from their respective marketed formulation. A detailed systemic survey of the sample preparation techniques, the chromatographic conditions and detection of the respective fluoroquinolones has been presented in this study. In the course of this discussion the advantages and applicability of the high performance liquid chromatographic techniques are also examined.

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“…Another option is to use Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction salts. This combination of different extraction procedures provides a high-throughput sample preparation with high recovery rates for a wide range of pH dependable analytes [129,130].…”

Section: (D) Sample Preparationmentioning

confidence: 99%

“…Recoveries are generally determined by comparing the analyte peak areas with those of reference samples after SPE. Alternatively, the sample can be spiked with an (isotopically labelled) internal standard prior to sample preparation [59,129,141].…”

Section: (D) Sample Preparationmentioning

confidence: 99%

Quantitative mass spectrometry methods for pharmaceutical analysis

Loos¹,

Schepdael²,

Cabooter³

2016

Phil. Trans. R. Soc. A.

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Quantitative pharmaceutical analysis is nowadays frequently executed using mass spectrometry. Electrospray ionization coupled to a (hybrid) triple quadrupole mass spectrometer is generally used in combination with solid-phase extraction and liquid chromatography. Furthermore, isotopically labelled standards are often used to correct for ion suppression. The challenges in producing sensitive but reliable quantitative data depend on the instrumentation, sample preparation and hyphenated techniques. In this contribution, different approaches to enhance the ionization efficiencies using modified source geometries and improved ion guidance are provided. Furthermore, possibilities to minimize, assess and correct for matrix interferences caused by co-eluting substances are described. With the focus on pharmaceuticals in the environment and bioanalysis, different separation techniques, trends in liquid chromatography and sample preparation methods to minimize matrix effects and increase sensitivity are discussed. Although highly sensitive methods are generally aimed for to provide automated multi-residue analysis, (less sensitive) miniaturized set-ups have a great potential due to their ability for in-field usage. This article is part of the themed issue ‘Quantitative mass spectrometry’.

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Multi-residue analysis of pharmaceuticals in aqueous environmental samples by online solid-phase extraction–ultra-high-performance liquid chromatography-tandem mass spectrometry: Optimisation and matrix effects reduction by quick, easy, cheap, effective, rugged and safe extraction

Cited by 84 publications

References 43 publications

Factors influencing the extraction of pharmaceuticals from sewage sludge and soil: an experimental design approach

Factors influencing the extraction of pharmaceuticals from sewage sludge and soil: an experimental design approach

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Quantitative mass spectrometry methods for pharmaceutical analysis

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