کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1165425 1491067 2013 9 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Isotope pattern deconvolution-tandem mass spectrometry for the determination and confirmation of diclofenac in wastewaters
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
Isotope pattern deconvolution-tandem mass spectrometry for the determination and confirmation of diclofenac in wastewaters
چکیده انگلیسی

Isotope dilution mass spectrometry (IDMS) based on isotope pattern deconvolution (IPD) has been applied here to MS/MS (QqQ) in order to carry out the quantification and confirmation of organic compounds in complex matrix water samples without the use of a methodological IDMS calibration graph. In this alternative approach, the isotope composition of the spiked sample is measured after fragmentation by SRM and deconvoluted into its constituting components (molar fractions of natural abundance and labeled compound) by multiple linear regression (IPD). The procedure has been evaluated for the determination of the pharmaceutical diclofenac in effluent and influent urban wastewaters and fortified surface waters by UHPLC (ESI) MS/MS using diclofenac-d4 as labeled compound. Calculations were performed acquiring a part and the whole fragment cluster ion, achieving in all cases recoveries within 90–110% and coefficients of variation below 5% for all water samples tested. In addition, potential false negatives arising from the presence of diclofenac-d2 impurities in the labeled compound were avoided when the proposed approach was used instead of the most usual IDMS calibration procedure. The number of SRM transitions measured was minimized to three to make possible the application of this alternative technique in routine multi-residue analysis.

Figure optionsDownload as PowerPoint slideHighlights
► Isotope dilution with isotope pattern deconvolution (IPD) has been applied to LC–MS/MS.
► The procedure allows the determination of organic compounds without calibration graph.
► Diclofenac determination in wastewater showed the need of this methodology in LC–MS/MS.
► Confirmation was accomplished with routine transitions used in multiresidue analysis.
► IPD permits the minimal labeling of the analyte which minimizes isotopic effect.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Analytica Chimica Acta - Volume 765, 26 February 2013, Pages 77–85
نویسندگان
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