Simultaneous determination of parabens, triclosan and triclocarban in water by liquid chromatography/electrospray ionisation tandem mass spectrometry.
A method for the determination of several household biocides in water by liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) is presented. It permits the simultaneous determination of triclosan (TCS), triclocarban (TCC) and seven parabens, including the distinction between branched and linear isomers of propyl (i-PrP and n-PrP) and butyl parabens (i-BuP and n-BuP). Prior to LC/MS/MS, analytes are preconcentrated by solid-phase extraction (SPE) on Oasis HLB (60 mg) cartridges at natural sample pH and subsequently eluted with 4 mL of methanol. This simple SPE procedure provides extraction recoveries above 85% except for raw wastewater, where it falls to 65% for TCC. The performance of the method was tested with two triple-quadrupole LC/MS instruments from a low/mid and mid/high market range: a Varian 1200L and an API-4000. The latter system provided between 3 and 80 times lower limits of quantification (LOQs) than the first one, in the 0.08-0.44 ng/L range for surface water. Moreover, a comparison of matrix effects on both instruments showed a very different behaviour, particularly in the case of parabens. For these compounds signal suppression was observed in the 1200L instrument and signal enhancement with the 4000 instrument. As a result, different calibration approaches were chosen for them and this pointed to the need of matrix effect re-evaluation in method transfer between different LC/MS systems. The application of the method to real samples showed the ubiquity of methyl paraben (MeP) and n-PrP (at the 1-6 microg/L in raw wastewater) and the coexistence of i-BuP and n-BuP at similar levels (ca. 100-200 ng/L in raw wastewater).
Department of Analytical Chemistry, Nutrition and Food Sciences, IIAA - Institute for Food Analysis and Research, University of Santiago de Compostela, 15782 Santiago de Compostela, Spain.
Iria
I
González-Mariño
José Benito
JB
Quintana
Isaac
I
Rodríguez
Rafael
R
Cela
D002224:Carbanilides / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D010226:Parabens / Q000032:analysis*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods; D014260:Triclosan / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis*
D002224:Carbanilides; D010226:Parabens; D014874:Water Pollutants, Chemical; D014260:Triclosan; C009540:triclocarban