PMID- 23932027 OWN - NLM STAT- MEDLINE DCOM- 20140218 LR - 20130820 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1307 DP - 2013 Sep 13 TI - Dispersive micro solid-phase extraction for the rapid analysis of synthetic polycyclic musks using thermal desorption gas chromatography-mass spectrometry. PG - 34-40 LID - S0021-9673(13)01134-5 [pii] LID - 10.1016/j.chroma.2013.07.074 [doi] AB - A simple and solvent-free method for the rapid analysis of five synthetic polycyclic musks in water samples is described. The method involves the use of dispersive micro solid-phase extraction (D-mu-SPE) coupled with direct thermal desorption (TD) gas chromatography-mass spectrometry (GC-MS) operating in the selected-ion-storage (SIS) mode. The parameters affecting the extraction efficiency of the target analytes from water sample and the thermal desorption conditions in the GC injection-port were optimized using a central composite design method. The optimal extraction conditions involved immersing 3.2mg of a typical octadecyl (C18) bonded silica adsorbent (i.e., ENVI-18) in a 10mL water sample. After extraction by vigorously shaking for 1.0min, the adsorbents were collected and dried on a filter. The adsorbents were transferred to a micro-vial, which was directly inserted into GC temperature-programmed injector, and the extracted target analytes were then thermally desorbed in the GC injection-port at 337 degrees C for 3.8min. The limits of quantitation (LOQs) were determined to be 1.2-3.0ng/L. Precision, as indicated by relative standard deviations (RSDs), was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 74 and 90%. A preliminary analysis of the river water samples revealed that galaxolide (HHCB) and tonalide (AHTN) were the two most common synthetic polycyclic musks present. Using a standard addition method, their concentrations were determined to in the range from 11 to 140ng/L. CI - Copyright (c) 2013 Elsevier B.V. All rights reserved. FAU - Chung, Wu-Hsun AU - Chung WH AD - Department of Chemistry, National Central University, Chung-Li 320, Taiwan; Department of Chemical Engineering, Army Academy ROC, Chung-Li 320, Taiwan. FAU - Tzing, Shin-Hwa AU - Tzing SH FAU - Ding, Wang-Hsien AU - Ding WH LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20130724 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Fatty Acids, Monounsaturated) RN - 0 (Polycyclic Compounds) RN - 0 (Water Pollutants, Chemical) RN - 095I377U8F (musk) SB - IM MH - Analysis of Variance MH - Fatty Acids, Monounsaturated/*analysis/isolation & purification MH - Gas Chromatography-Mass Spectrometry/*methods MH - Limit of Detection MH - Linear Models MH - Polycyclic Compounds/*analysis/isolation & purification MH - Reproducibility of Results MH - Rivers/chemistry MH - Solid Phase Microextraction/*methods MH - Water Pollutants, Chemical/analysis/isolation & purification OTO - NOTNLM OT - Dispersive micro solid-phase extraction OT - Synthetic musks OT - Thermal desorption-GC-MS OT - Water analysis EDAT- 2013/08/13 06:00 MHDA- 2014/02/19 06:00 CRDT- 2013/08/13 06:00 PHST- 2013/03/17 00:00 [received] PHST- 2013/07/18 00:00 [revised] PHST- 2013/07/18 00:00 [accepted] PHST- 2013/08/13 06:00 [entrez] PHST- 2013/08/13 06:00 [pubmed] PHST- 2014/02/19 06:00 [medline] AID - S0021-9673(13)01134-5 [pii] AID - 10.1016/j.chroma.2013.07.074 [doi] PST - ppublish SO - J Chromatogr A. 2013 Sep 13;1307:34-40. doi: 10.1016/j.chroma.2013.07.074. Epub 2013 Jul 24.