| 摘要: | 摘要: An optimized method for the determination of two major carbon‐based engineered nanoparticles (C60 and C70) in marketed fish samples is described. The method involves the use of microwave‐assisted extraction (MAE) coupled with liquid chromatography ‐ tandem mass spectrometry with atmospheric pressure photoionization (LC‐APPI‐MS/MS). Factors affecting the extraction efficiency of the analytes from fish samples were optimized by a central composite design method. The optimal extraction temperature and time for MAE were found to be 233 °C for 22 min, and the extraction solution was composed of toluene and acetone in a ratio of 4.64:1. The limits of quantitation (LOQs) were 0.1 and 0.05 ng/g for C60 and C70, respectively. The precision for these analytes at two spiked levels, as indicated by relative standard deviations (RSDs), were less than 10% for both intra‐ and inter‐day analysis. Accuracy, expressed as the mean extraction recovery, was between 85 and 98%. The method was further validated based on EU Commission Decision 2002/657/EC, including a decision limit (CCα) and detection capability (CCβ) for marketed fish samples. A high throughput and reliable MAE technique coupled with LC‐APPI‐MS/MS was developed to determine two major carbon‐based ENPs, C60 and C70, in marketed fish samples. The developed method provides good precision, a wide range of linearity, and detection limits at the sub‐ng/g level when analyzing fish samples. 其他題名: Jnl Chinese Chemical Soc 出版者: Weinheim: WILEY-VCH Verlag 出版日期: 2014-03 出處: Journal of the Chinese Chemical Society (Taipei), 2014-03, Vol.61 (3), p.350-356 版權: Copyright © 2014 The Chemical Society Located in Taipei & Wiley‐VCH Verlag GmbH & Co. KGaA, Weinheim, Germany 版權: Copyright © 2014 The Chemical Society Located in Taipei & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim, Germany 識別號: ISSN: 0009-4536 識別號: EISSN: 2192-6549 識別號: DOI: 10.1002/jccs.201300356 |