PMID- 22981507 OWN - NLM STAT- MEDLINE DCOM- 20130107 LR - 20120926 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1260 DP - 2012 Oct 19 TI - Planar solid phase extraction clean-up for pesticide residue analysis in tea by liquid chromatography-mass spectrometry. PG - 42-53 LID - S0021-9673(12)01339-8 [pii] LID - 10.1016/j.chroma.2012.08.088 [doi] AB - Efficient clean-up is indispensable for preventing matrix effects in multi-residue analysis of pesticides in food by liquid and gas chromatography (LC and GC) coupled to mass spectrometry (MS). High-throughput planar solid phase extraction (HTpSPE) was recently introduced as a new clean-up concept in residue analysis of pesticides in fruit and vegetables (C. Oellig, W. Schwack, 2011 [45]). Thin-layer chromatography (TLC) was used to completely separate pesticides from matrix compounds and to focus them into a sharp zone, followed by extraction of the target zone by the TLC-MS interface. As rather challenging matrices, tea samples were chosen in this study. Besides chlorophylls and polyphenols, high amount of caffeine is co-extracted resulting in strong matrix effects both in LC-MS and GC-MS. The former HTpSPE procedure was adapted to initial extracts of green and black tea resulting in colorless extracts nearly free of matrix effects and interferences, as shown for seven chemically representative pesticides (acetamiprid, penconazole, azoxystrobin, chlorpyrifos, pirimicarb, fenarimol, and mepanipyrim). LC-MS/MS calibration curves obtained in the range of 0.002-0.5 mg/kg from matrix-matched standards and solvent standards were nearly identical and demonstrated the effectiveness of clean-up by HTpSPE. Mean recoveries determined by LC-MS/MS against solvent standards at spiking levels of 0.01 and 0.1 mg/kg ranged between 72 and 114% with relative standard deviations (RSDs) of 0.7-4.7% (n=4), while LC-MS measurements of tea samples spiked at 1 mg/kg provided recoveries of 81-104% with RSDs of 1.2-4.9% (n=6). Using LC-MS/MS, the method showed high sensitivity with signal-to-noise ratios>10 for concentrations below 0.002 mg/kg. HTpSPE of one sample was done in a few minutes, while numerous samples were cleaned in parallel at minimal costs with very low sample and solvent consumption. CI - Copyright (c) 2012 Elsevier B.V. All rights reserved. FAU - Oellig, Claudia AU - Oellig C AD - Institute of Food Chemistry, University of Hohenheim, Garbenstrasse 28, 70599 Stuttgart, Germany. claudia.oellig@uni-hohenheim.de FAU - Schwack, Wolfgang AU - Schwack W LA - eng PT - Journal Article DEP - 20120901 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Pesticide Residues) RN - 0 (Tea) SB - IM MH - Chromatography, Thin Layer/*methods MH - Linear Models MH - Mass Spectrometry/*methods MH - Pesticide Residues/analysis/*isolation & purification MH - Reproducibility of Results MH - Signal-To-Noise Ratio MH - Solid Phase Extraction/*methods MH - Tea/*chemistry EDAT- 2012/09/18 06:00 MHDA- 2013/01/08 06:00 CRDT- 2012/09/18 06:00 PHST- 2012/06/28 00:00 [received] PHST- 2012/08/27 00:00 [revised] PHST- 2012/08/29 00:00 [accepted] PHST- 2012/09/18 06:00 [entrez] PHST- 2012/09/18 06:00 [pubmed] PHST- 2013/01/08 06:00 [medline] AID - S0021-9673(12)01339-8 [pii] AID - 10.1016/j.chroma.2012.08.088 [doi] PST - ppublish SO - J Chromatogr A. 2012 Oct 19;1260:42-53. doi: 10.1016/j.chroma.2012.08.088. Epub 2012 Sep 1.