PMID- 22209304 OWN - NLM STAT- MEDLINE DCOM- 20120307 LR - 20191210 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1223 DP - 2012 Feb 3 TI - Determination of aqueous fullerene aggregates in water by ultrasound-assisted dispersive liquid-liquid microextraction with liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry. PG - 15-23 LID - 10.1016/j.chroma.2011.12.034 [doi] AB - A simple and solvent-minimized method for the determination of three aqueous fullerene aggregates (nC(6)(0), nC(7)(0), and aqueous [6,6]-phenyl C(6)(1) butyric acid methyl ester (nPCBM)) in water samples is described. The method involves the use of ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled liquid chromatography-tandem mass spectrometry with atmospheric pressure photoionization (LC-APPI-MS/MS). The parameters affecting the extraction efficiency of the analytes from water samples were systematically investigated and the conditions optimized. The best extraction conditions involved the rapid injection of a mixture of 1.0 mL of 2-propanol (as a disperser solvent) and 10 muL of benzyl bromide (as an extraction solvent) into 10 mL of an aqueous solution (pH 10.0) containing 1% sodium chloride in a conical bottom glass tube. After ultrasonication for 1.0 min and centrifugation at 5000 pm (10 min), the sedimented phase 5.0 muL was directly injected into the LC-APPI-MS/MS system. The limits of quantification (LOQs) were 150, 60 and 8 ng L(-)(1) for nPCBM, nC(6)(0) and nC(7)(0), respectively. The precision for these analytes, as indicated by relative standard deviations (RSDs), were less than 12% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 70 and 86%. A standard addition method was used to quantitate three aqueous fullerene aggregates, and the concentrations of these aqueous fullerene aggregates were determined to be in the range from n.d. to 130 ng L(-)(1) in various environmental samples including municipal influent and effluent samples, industrial wastewater samples, and surface water samples. CI - Copyright (c) 2011 Elsevier B.V. All rights reserved. FAU - Chen, Hsin-Chang AU - Chen HC AD - Department of Chemistry, National Central University, Chung-Li 320, Taiwan. FAU - Ding, Wang-Hsien AU - Ding WH LA - eng PT - Evaluation Study PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20111214 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Fullerenes) RN - 0 (Water Pollutants) RN - 059QF0KO0R (Water) SB - IM MH - Fullerenes/analysis/*isolation & purification MH - Liquid Phase Microextraction/economics/*methods MH - Sensitivity and Specificity MH - Tandem Mass Spectrometry/economics/methods MH - Ultrasonics/economics/methods MH - Water/*analysis MH - Water Pollutants/analysis/*isolation & purification EDAT- 2012/01/03 06:00 MHDA- 2012/03/08 06:00 CRDT- 2012/01/03 06:00 PHST- 2011/07/28 00:00 [received] PHST- 2011/12/07 00:00 [revised] PHST- 2011/12/08 00:00 [accepted] PHST- 2012/01/03 06:00 [entrez] PHST- 2012/01/03 06:00 [pubmed] PHST- 2012/03/08 06:00 [medline] AID - S0021-9673(11)01818-8 [pii] AID - 10.1016/j.chroma.2011.12.034 [doi] PST - ppublish SO - J Chromatogr A. 2012 Feb 3;1223:15-23. doi: 10.1016/j.chroma.2011.12.034. Epub 2011 Dec 14.