PMID- 17613050 OWN - NLM STAT- MEDLINE DCOM- 20071119 LR - 20131121 IS - 0265-203X (Print) IS - 0265-203X (Linking) VI - 24 IP - 7 DP - 2007 Jul TI - Determination of acrylamide in coffee and chocolate by pressurised fluid extraction and liquid chromatography-tandem mass spectrometry. PG - 663-72 AB - A selective and sensitive procedure has been developed and validated for the determination of acrylamide in difficult matrices, such as coffee and chocolate. The proposed method includes pressurised fluid extraction (PFE) with acetonitrile, florisil clean-up purification inside the PFE extraction cell and detection by liquid chromatography (LC) coupled to atmospheric pressure ionisation in positive mode tandem mass spectrometry (APCI-MS-MS). Comparison of ionisation sources (atmospheric pressure chemical ionisation (APCI), atmospheric pressure photoionization (APPI) and the combined APCI/APPI) and clean-up procedures were carried out to improve the analytical signal. The main parameters affecting the performance of the different ionisation sources were previously optimised using statistical design of experiments (DOE). PFE parameters were also optimised by DOE. For quantitation, an isotope dilution approach was used. The limit of quantification (LOQ) of the method was 1 microg kg(-1) for coffee and 0.6 microg kg(-1) for chocolate. Recoveries ranged between 81-105% in coffee and 87-102% in chocolate. The accuracy was evaluated using a coffee reference test material FAPAS T3008. Using the optimised method, 20 coffee and 15 chocolate samples collected from Valencian (Spain) supermarkets, were investigated for acrylamide, yielding median levels of 146 microg kg(-1) in coffee and 102 microg kg(-1) in chocolate. FAU - Pardo, O AU - Pardo O AD - Public Health Laboratory of Valencia, Generalitat Valenciana, Valencia, Spain. FAU - Yusa, V AU - Yusa V FAU - Coscolla, C AU - Coscolla C FAU - Leon, N AU - Leon N FAU - Pastor, A AU - Pastor A LA - eng PT - Journal Article PL - England TA - Food Addit Contam JT - Food additives and contaminants JID - 8500474 RN - 0 (Coffee) RN - 20R035KLCI (Acrylamide) SB - IM MH - Acrylamide/*analysis MH - Cacao/*chemistry MH - Chromatography, Liquid/methods MH - Coffee/*chemistry MH - Spain MH - Tandem Mass Spectrometry/methods EDAT- 2007/07/07 09:00 MHDA- 2007/12/06 09:00 CRDT- 2007/07/07 09:00 PHST- 2007/07/07 09:00 [pubmed] PHST- 2007/12/06 09:00 [medline] PHST- 2007/07/07 09:00 [entrez] AID - 779724068 [pii] AID - 10.1080/02652030701235198 [doi] PST - ppublish SO - Food Addit Contam. 2007 Jul;24(7):663-72. doi: 10.1080/02652030701235198.