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Analysis of organophosphate pesticides in surface water—Comparison of method optimization approaches
Author(s) -
Habedank Friederike,
Feldhusen Frerk,
SchulzBull Detlef,
Kanwischer Marion
Publication year - 2020
Publication title -
journal of chemometrics
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.47
H-Index - 92
eISSN - 1099-128X
pISSN - 0886-9383
DOI - 10.1002/cem.3220
Subject(s) - chromatography , chemistry , extraction (chemistry) , taguchi methods , design of experiments , sample preparation , acetone , methanol , mass spectrometry , response surface methodology , analytical chemistry (journal) , mathematics , statistics , organic chemistry
A multiresidue method optimization was conducted using the design of experiment approach. Out of 43 tested organophosphate compounds, 27 could be validated in surface water, yielding limits of detection of 0.6 to 2.5 ng L− 1by dispersive liquid‐liquid micro‐extraction and subsequent liquid chromatography‐tandem quadrupole mass spectrometry (LC‐MSMS) detection. For the optimization of the sample preparation, the factors sonication time, sample volume, binary extraction ratio, and addition of salt have been investigated by the Taguchi design of experiment approach. One hundred fifty milliliters sample were extracted for 1 minute with 400 μ L acetone and 800 μ L tetrachloroethene (TCE) three times subsequently. No salts were added. Combined extracts were reconstituted in 65 μ L methanol, ready for analysis. The design of experiment approach for method optimization is discussed thoroughly. The comparison to one factor at a time approach focuses on overall experimental expenditure, factor space coverage, acquired information regarding factor interactions, and statistical confirmation of results. Based on two similar analytical methods, it is illustrated that fewer but statistically derived experiments yield more information about the overall system enabling enhanced evaluation of experiment results.