TY - JOUR
T1 - Analysis of pharmaceuticals in fish using liquid chromatography-tandem mass spectrometry
AU - Ramirez, Alejandro J.
AU - Mottaleb, Mohammad A.
AU - Brooks, Bryan W.
AU - Chambliss, C. Kevin
PY - 2007/4/15
Y1 - 2007/4/15
N2 - A liquid chromatography-tandem mass spectrometry (LC-MS/MS) screening method has been developed targeting 23 pharmaceuticals and 2 metabolites with differing physicochemical properties in fish tissue. Reversed-phase separation of target compounds was achieved using a C18 column and a nonlinear gradient consisting of 0.1% (v/v) formic acid and methanol. Eluted analytes were introduced into the mass analyzer using positive or negative electrospray ionization, as appropriate. A variety of extraction solvents, differing in polarity, pH, or both, were investigated in order to assess recovery of target compounds from 1-g tissue homogenates. Among 10 solvents tested, a 1:1 mixture of 0.1 M aqueous acetic acid (pH 4) and methanol was identified as optimal, resulting in extraction recoveries for 24 of 25 compounds exceeding 60%. Tissue extracts were found to influence the LC-MS/MS response for several analytes. Consequently, matrix-matched calibration standards were employed to determine analyte concentrations in environmental samples. Statistically derived method detection limits were <6 ng/g for most analytes. The method was subsequently used to screen for target analytes in fish from an effluent-dominated stream. Diphenhydramine, diltiazem, carbamazepine, and norfluoxetine were detected in 11 of 11 environmental samples at concentrations ranging from 0.11 to 5.14 ng/g.
AB - A liquid chromatography-tandem mass spectrometry (LC-MS/MS) screening method has been developed targeting 23 pharmaceuticals and 2 metabolites with differing physicochemical properties in fish tissue. Reversed-phase separation of target compounds was achieved using a C18 column and a nonlinear gradient consisting of 0.1% (v/v) formic acid and methanol. Eluted analytes were introduced into the mass analyzer using positive or negative electrospray ionization, as appropriate. A variety of extraction solvents, differing in polarity, pH, or both, were investigated in order to assess recovery of target compounds from 1-g tissue homogenates. Among 10 solvents tested, a 1:1 mixture of 0.1 M aqueous acetic acid (pH 4) and methanol was identified as optimal, resulting in extraction recoveries for 24 of 25 compounds exceeding 60%. Tissue extracts were found to influence the LC-MS/MS response for several analytes. Consequently, matrix-matched calibration standards were employed to determine analyte concentrations in environmental samples. Statistically derived method detection limits were <6 ng/g for most analytes. The method was subsequently used to screen for target analytes in fish from an effluent-dominated stream. Diphenhydramine, diltiazem, carbamazepine, and norfluoxetine were detected in 11 of 11 environmental samples at concentrations ranging from 0.11 to 5.14 ng/g.
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U2 - 10.1021/ac062215i
DO - 10.1021/ac062215i
M3 - Article
C2 - 17348635
AN - SCOPUS:34247346615
VL - 79
SP - 3155
EP - 3163
IS - 8
ER -