Dispersive micro solid-phase extraction for the rapid analysis of synthetic polycyclic musks using thermal desorption gas chromatography-mass spectrometry.
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 3.2mg 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°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.
Department of Chemistry, National Central University, Chung-Li 320, Taiwan; Department of Chemical Engineering, Army Academy ROC, Chung-Li 320, Taiwan.
Wu-Hsun
WH
Chung
Shin-Hwa
SH
Tzing
Wang-Hsien
WH
Ding
D000704:Analysis of Variance; D005229:Fatty Acids, Monounsaturated / Q000032:analysis* / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D016014:Linear Models; D011083:Polycyclic Compounds / Q000032:analysis* / Q000302:isolation & purification; D015203:Reproducibility of Results; D045483:Rivers / Q000737:chemistry; D052617:Solid Phase Microextraction / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000302:isolation & purification
D005229:Fatty Acids, Monounsaturated; D011083:Polycyclic Compounds; D014874:Water Pollutants, Chemical; C008563:musk
Dispersive micro solid-phase extraction; Synthetic musks; Thermal desorption-GC–MS; Water analysis