Solid-phase dynamic extraction

Use of Automated Solid Phase Dynamic Extraction (SPDE)/GC-MS and Novel Macros in the Search for African Elephant Pheromones ... 

Abstract A relatively small number of mammalian pheromones has been identified, in contrast to a plethora of known insect pheromones, but two remarkable Asian elephant/insect pheromonal linkages have been elucidated, namely, (Z)-7-dodecen-1-yl acetate and frontalin. In addition, behavioral bioassays have demonstrated the presence of a chemical signal in the urine of female African elephants around the time of ovulation. Our search for possible ovulatory pheromones in the headspace over female African elephant urine has revealed for the first time the presence of a number of known insect pheromones. This search has been facilitated by the use of a powerful new analytical technique, automated solid phase dynamic extraction (SPDE)/GC-MS, as well as by novel macros for enhanced and rapid comparison of multiple mass spectral data files from Agilent ChemStation . This chapter will focus on our methodologies and results, as well as on a comparison of SPDE and the more established techniques of solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). 

Automated Solid Phase Dynamic Extraction (SPDE)... 

Bicchi, C., Cordero, C., Liberto, E., Rubiolo, P. and Sgorbini, B. (2004) Automated headspace solid-phase dynamic extraction to analyse the volatile fraction of food matrices. J. Chromatogr. A 1024, 217-226. 

Lipinski, J. (2001) Automated solid phase dynamic extraction-Extraction of organics using a wall coated syringe needle. Fresenius J. Anal. Chem. 369, 57-62. 

Musshoff, F., Lachenmeier, D.W., Kroener, L. and Madea, B. (2002) Automated headspace solid-phase dynamic extraction for the determination of amphetamines and synthetic designer drugs in hair samples. J. Chromatogr. A 958, 231-238. 

Goodwin, T.E., Brown, P., Eggert, M., Evola, M., House, S., Morshedi, G., Weddell, M., Chen, J., Jackson, S.R., Aubut, Y., Eggert, J., Schulte, B.A. and Rasmussen, L.E.L. (2007) Use of automated solid phase dynamic extraction (SPDE)/GC-MS and novel macros in the search for African elephant pheromones. In J. Hurst, R. Beynon C. Roberts and T. Wyatt (Eds.), Chemical Signals in Vertebrates 11. Springer Press, New York, pp. 20-29. 

Antebrachial secretions were comprised primarily of low-molecular weight compounds. Because of the high volatility of these secretions, we could not produce reliable chromatograms using our routine extraction procedure. We are currently analyzing these secretions using solid phase dynamic extraction techniques (in col-... 

Membrane SLM MESI MMLLE MIMS PME HF-LPME MASE LGLME Headspace-solid phase dynamic extraction (HS-SPDE) Purge-and-membrane extraction Headspace/membrane extraction w. sorbent interface (HS-MESI) Headspace/membrane inlet mass spectrometry (HS-MIMS)... 

SPDE tubular microextraction Solid-phase dynamic extraction with sol-gel coating of more polar analytes... 

Van Durme, J., Demeestere, K., Dewulf, J., Ronsse, F., Braeckman, L., Pieters, J., Van Langenhove, H. Accelerated solid-phase dynamic extraction of toluene from air. J. Chromatogr. A 1175, 145-153 (2007)... 

Laaks, J., Letzel, T., Schmidt, T.C., Jochmann, M.A. Fingerprinting of red wine by head-space solid-phase dynamic extraction of volatile constituents. Anal. Bioanal. Chem. 403, 2429-2436 (2012)... 

Fig.l Headspace analysis and microextraction methods (here only the headspace mode is shown) used for the determination of fuel oxygenates, (a) Headspace analysis, (b) headspace solid-phase microextraction (HS-SPME) redrawn after [60], (c) solid-phase dynamic extraction (SPDE) redrawn after [61] and (d) liquid-phase microextraction (LPME) redrawn after [62]... 

As shown in Fig. Ic, solid-phase dynamic extraction (SPDE) utilizes a 2.5 mL headspace syringe with a needle that is coated on the inside similar to a fused silica GC column with an immobilized extraction phase. SPDE needle coat-... 

M. B. Gholivand, M. M. Abolghasemi, Inside needle capillary adsorption trap device for headspace solid-phase dynamic extraction based on polyaniline/ hexagonally ordered silica nanocomposite. / Sep Sci 2012,35 (5-6), 695-701. 

The search of adequate extraction techniques allowing the identification and quantification of wine volatile compounds has attracted the attention of many scientists. This has resulted in the availability of a wide range of analytical tools for the extraction of these compounds from wine. These methodologies are mainly based on the solubility of the compounds in organic solvents (liquid-liquid extraction LLE, simultaneous distillation liquid extraction SDE), on their volatility (static and dynamic headspace techniques), or based on their sorptive/adsorptive capacity on polymeric phases (solid phase extraction SPE, solid phase microextraction SPME, stir bar sorptive extraction SBSE). In addition, volatile compounds can be extracted by methods based on combinations of some of these properties (headspace solid phase microextraction HS-SPME, solid phase dynamic extraction SPDE). 

Bagheri, H. Babanezhad, E. Khalilian, F. (2009). An Interior Needle Electropolymerized Pyrrole-Based Coating for Headspace Solid-Phase Dynamic Extraction. Anal. Chim. Acta, Vol.634, pp. 209-214, ISSN 00032670. 

Musshoff, F. Lachenmeier, D. Kroener, L. Madea, B. (2003). Automated Headspace Solid-Phase Dynamic Extraction for the Determination of Cannabinoids in Hair Samples. Forensic Sci Int, Vol.133, pp. 32-38, ISSN 03790738. 

KAM 07] Kamphoff M., Thiele T., Kunz B., Influence of different extraction parameter on a solid-phase dynamic extraction for the gas chromatographic determination of d-limonene degradation products by using a fractional factorial design . Journal ofAOACInternational, vol. 90, pp. 1623-2627, 2007. 

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