Multi-residue analytical method for human pharmaceuticals and synthetic hormones in river water and sewage effluents by solid-phase extraction and liquid chromatography-tandem mass spectrometry

Najat Ahmed Al-Odaini, Mohamad Pauzi Zakaria, Mohamad Ismail Yaziz, Salmijah Surif

    Research output: Contribution to journalArticle

    135 Citations (Scopus)

    Abstract

    Pollutants such as human pharmaceuticals and synthetic hormones that are not covered by environmental legislation have increasingly become important emerging aquatic contaminants. This paper reports the development of a sensitive and selective multi-residue method for simultaneous determination and quantification of 23 pharmaceuticals and synthetic hormones from different therapeutic classes in water samples. Target pharmaceuticals include anti-diabetic, antihypertensive, hypolipidemic agents, β2-adrenergic receptor agonist, antihistamine, analgesic and sex hormones. The developed method is based on solid phase extraction (SPE) followed by instrumental analysis using liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) with 30min total run time. River water samples (150mL) and (sewage treatment plant) STP effluents (100mL) adjusted to pH 2, were loaded into MCX (3cm3, 60mg) cartridge and eluted with four different reagents for maximum recovery. Quantification was achieved by using eight isotopically labeled internal standards (I.S.) that effectively correct for losses during sample preparation and matrix effects during LC-ESI-MS/MS analysis. Good recoveries higher than 70% were obtained for most of target analytes in all matrices. Method detection limit (MDL) ranged from 0.2 to 281ng/L. The developed method was applied to determine the levels of target analytes in various samples, including river water and STP effluents. Among the tested emerging pollutants, chlorothiazide was found at the highest level, with concentrations reaching up to 865ng/L in STP effluent, and 182ng/L in river water.

    Original languageEnglish
    Pages (from-to)6791-6806
    Number of pages16
    JournalJournal of Chromatography A
    Volume1217
    Issue number44
    DOIs
    Publication statusPublished - 29 Oct 2010

    Fingerprint

    Solid Phase Extraction
    Liquid chromatography
    Sewage
    Tandem Mass Spectrometry
    Rivers
    Liquid Chromatography
    Mass spectrometry
    Effluents
    Hormones
    Water
    Pharmaceutical Preparations
    Chlorothiazide
    Hypolipidemic Agents
    Recovery
    Sewage treatment plants
    Electrospray ionization
    Adrenergic Agonists
    Electrospray Ionization Mass Spectrometry
    Histamine Antagonists
    Gonadal Steroid Hormones

    Keywords

    • Aquatic pollution
    • Human pharmaceuticals
    • Liquid chromatography-tandem mass spectrometry (LC-MS/MS)
    • Malaysia
    • Multi-residue analytical method
    • Solid phase extraction (SPE)
    • Synthetic hormones

    ASJC Scopus subject areas

    • Analytical Chemistry
    • Organic Chemistry
    • Biochemistry

    Cite this

    Multi-residue analytical method for human pharmaceuticals and synthetic hormones in river water and sewage effluents by solid-phase extraction and liquid chromatography-tandem mass spectrometry. / Al-Odaini, Najat Ahmed; Zakaria, Mohamad Pauzi; Yaziz, Mohamad Ismail; Surif, Salmijah.

    In: Journal of Chromatography A, Vol. 1217, No. 44, 29.10.2010, p. 6791-6806.

    Research output: Contribution to journalArticle

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