Dispersive micro solid-phase extraction for the rapid analysis of synthetic polycyclic musks using thermal desorption gas chromatography-mass spectrometry

Wu Hsun Chung, Shin Hwa Tzing, Wang Hsien Ding

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42 Scopus citations

Abstract

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-μ-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 3.2. mg of a typical octadecyl (C18) bonded silica adsorbent (i.e., ENVI-18) in a 10. mL water sample. After extraction by vigorously shaking for 1.0. min, 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. °C for 3.8. min. The limits of quantitation (LOQs) were determined to be 1.2-3.0. ng/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 140. ng/L.

Original languageEnglish
Pages (from-to)34-40
Number of pages7
JournalJournal of Chromatography A
Volume1307
DOIs
StatePublished - 13 Sep 2013

Keywords

  • Dispersive micro solid-phase extraction
  • Synthetic musks
  • Thermal desorption-GC-MS
  • Water analysis

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