A New SPME Thermal Desorption Interface for HPLC


A new SPME/HPLC interface is developed. It is based on thermal desorption from the SPME fiber and organic solvent collection of the desorbed analytes by sweeping them with an argon flow into a small organic solvent volume which is further injected into the HPLC chromatograph. Extraction and desorption parameters were investigated using five PAHs of different volatilities (naphthalene, acenaphthalene, fluorene, phenanthrene and anthracene) as test compounds and fluorimetric detection. Regression coefficients closed to 0.99 with RDS < 14% (n = 3) and detection limits in the range 0.07 - 0.99 μg.L-1 were found. A method was applied to determine the above PAHs in water samples. The results were compared with those supplied by the 550.1 EPA method showing the agreement of both methods at the 0.05 significance level.

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J. Acevedo, M. Sayadi and L. Díez, "A New SPME Thermal Desorption Interface for HPLC," Journal of Analytical Sciences, Methods and Instrumentation, Vol. 3 No. 4, 2013, pp. 219-266. doi: 10.4236/jasmi.2013.34028.

Conflicts of Interest

The authors declare no conflicts of interest.


[1] Z. Mester, R. Sturgeon and J. Pawliszyn, “Solid Phase Microextraction as a Tool for Trace Element Speciation,” Spectrochimica Acta Part B: Atomic Spectroscopy, Vol. 56, No. 3, 2001, pp. 233-260.
[2] Y. Fan, Y. Feng, T. Zhang, S. Da and M. Zhang, “Poly (Methacrylic Acid-Ethylene Glycol Dimethacrylate) Monolith In-Tube Solid Phase Microextraction Coupled to High Performance Liquid Chromatography and Analysis of Amphetamines in Urine Samples,” Journal of Chromatography A, Vol. 1074, No. 1, 2005, pp. 9-16
[3] R. P. Belardi and J. Pawliszyn, “The application of chemically modified fused silica fibers in the extraction of organics from water matrix samples and their rapid transfer to capillary columns,” Water Pollution Research Journal of Canada, Vol. 24, 1989, pp. 179-191.
[4] M. N. Kayali, S. Rubio, M. P. Cuesta and L. M. Polo, “Rapid Determination of Polycyclic Aromatic Hydrocarbons in Tea Infusion Samples by High-Performance Liquid Chromatography and Fluorimetric Detection Based on Solid-Phase Extraction,” Analyst, Vol. 123, No. 10, 1998, pp. 2145-2148.
[5] A. Penalver, E. Pocurull, F. Borrull and R. M. Marcé, “Method Based on Solid-Phase Microextraction—High-Performance Liquid Chromatography with UV and Electrochemical Detection to Determine Estrogenic Compounds in Water Samples,” Journal of Chromatography A, Vol. 964, No. 1-2, 2002, pp. 153-160.
[6] Y. Wang, J. Zhang, et al., “Quantitative Determination of 16 Polycyclic Aromatic Hydrocarbons in Soil Samples Using Solid-Phase Microextraction,” Journal of Separation Science, Vol. 32, No. 22, 2009, pp. 3951-3957.
[7] Gaurav, A. K. Malik and P. K. Rai, “Development of a New SPME-HPLC-UV Method for the Analysis of Nitro Explosives on Reverse Phase Amide Column and Application to Analysis of Aqueous Samples,” Journal of Hazardous Materials, Vol. 172, No. 2-3, 2009, pp. 1652-1658. http://dx.doi.org/10.1016/j.jhazmat.2009.08.039
[8] R. J. Bartelt, “Calibration of a Commercial Solid-Phase Microextraction Device for Measuring Headspace Concentrations of Organic Volatiles,” Analytical Chemistry, Vol. 69, No. 3, 1997, pp. 364-372.
[9] C. Arthur and J. Pawliszyn, “Solid Phase Microextraction with Thermal Desorption Using Fused Silica Optical Fibers,” Analytical Chemistry, Vol. 62, No. 19, 1990, pp. 2145-2148. http://dx.doi.org/10.1021/ac00218a019
[10] M. R. Negrao and M. F. Alpendurada, “Solvent-Free Method for the Determination of Polynuclear Aromatic Hydrocarbons in Waste Water by Solid-Phase Microextraction-High-Performance Liquid Chromatography with Photodiode-Array Detection,” Journal of Chromatography A, Vol. 823, No. 1-2, 1998, pp. 211-218.
[11] K. Hiroyuki, “Recent Advances in Solid-Phase Microextraction and Related Techniques for Pharmaceutical and Biomedical Analysis,” Current Pharmaceutical Analysis, Vol. 1, No. 1, 2005, pp. 65-84.
[12] M. E. Miller and J. D. Stuart, “Comparison of Gas-Sampled and SPME-Sampled Static Headspace for the Determination of Volatile Flavor Components,” Analytical Chemistry, Vol. 71, No. 1, 1999, pp. 23-27.
[13] O. Ezquerro and M. Tena, “Determination of Odour-Causing Volatile Organic Compounds in Cork Stoppers by Multiple Headspace Solid-Phase Microextraction,” Journal of Chromatography A, Vol. 1068, No. 2, 2005, pp. 201-208. http://dx.doi.org/10.1016/j.chroma.2005.01.089
[14] W. Zhang and C. Zlin, “Mussel Inspired Polydopamine Functionalized Poly (Ether Ether Ketone) Tube for Online Solid-Phase Microextraction—High Performance Liquid Chromatography and Its Application in Analysis of Protoberberine Alkaloids in Rat Plasma,” Journal of Chromatography A, Vol. 1278, 2013, pp. 29-36.
[15] A. Bordagaray, R. García and E. Millán, “Development and Application of a Screening Method for Triazole Fungicide Determination in Liquid and Fruit Samples Using Solid-Phase Microextraction and HPLC-DAD,” Analytical Methods, Vol. 5, No. 10, 2013, pp. 2565-2571.
[16] S. Panseri, S. Soncin, L. M. Chiesa and P. A. Biondi, “A Headspace Solid-Phase Microextraction Gas-Chromatographic Mass-Spectrometric Method (HS-SPME-GC/MS) to Quantify Hexanal in Butter during Storage as Marker of Lipid Oxidation,” Food Chemistry, Vol. 127, No. 2, 2011, pp. 886-889.
[17] M. Tankiewicz, C. Morrison and M. Biziuk, “Application and Optimization of Headspace Solid-Phase Microextraction (HS-SPME) Coupled with Gas Chromatography-Flame-Ionization Detector (GC-FID) to Determine Products of the Petroleum Industry in Aqueous Samples,” Microchemical Journal, Vol. 108, 2013, pp. 117-123.
[18] Q. L. Ma, N. Hamid, A. E. D. Bekhit, J. Robertson and T. F. Law, “Optimization of Headspace Solid Phase Microextraction (HS-SPME) for Gas Chromatography Mass Spectrometry (GC-MS) Analysis of Aroma Compounds in Cooked Beef Using Response Surface Methodology,” Microchemical Journal, Vol. 111, 2013, pp. 16-24.
[19] Gaurav, V. Kaur, A. Kumar, A. Kumar and P. K. Rai, “SPME-HPLC: A New Approach to the Analysis of Explosives,” Journal of Hazardous Materials, Vol. 147, No. 3, 2007, pp. 691-697.
[20] C. Fernandes, A. J. dos Santos Neto, J. C. Rodrigues, C. Alves and F. Mauro Lancas, “Solid-Phase Microextraction-Liquid Chromatography (SPME-LC) Determination of Fluoxetine and Norfluoxetine in Plasma Using a Heated Liquid Flow through Interface,” Journal of Chromatography B, Vol. 847, No. 2, 2007, pp. 217-223.
[21] L. Cárdenes, J. Ayala, M. A. Afonso and V. González, “Solid-Phase Microextraction Coupled with High-Performance Liquid Chromatography for the Analysis of Heterocyclic Aromatic Amines,” Journal of Chromatography A, Vol. 1030, No. 1-2, 2004, pp. 87-93.
[22] H. Kataoka and K. Saito, “Recent Advances in SPME Techniques in Biomedical Analysis,” Journal of Pharmaceutical and Biomedical Analysis, Vol. 54, 2011, pp. 926-950.
[23] J. S. Aulakh, A. K. Malik, V. Kaur and P. M. Kopplin, “A Review on Solid Phase Micro Extraction—High Performance Liquid Chromatography (SPME-HPLC) Analysis of Pesticides,” Critical Reviews in Analytical Chemistry, Vol. 35, No. 1, 2005, pp. 71-85.
[24] N. Kayali, F. G. Tamayo and L. M. Polo, “Determination of Diethylhexyl Phtalate in Water by Solid Phase Microextraction Coupled to High Performance Liquid Chromatography,” Talanta, Vol. 69, No. 5, 2006, pp. 1095-1099. http://dx.doi.org/10.1016/j.talanta.2005.12.016
[25] H. L. Lord, “Strategies for Interfacing Solid-Phase Microextraction with Liquid Chromatography,” Journal of Chromatography A, Vol. 1152, No. 1, 2007, pp. 2-13.
[26] M. N. Kayali-Sayadi, J. M. Bautista, L. M. Polo-Díez and I. Salazar, “Identification of Pheromones in Mouse Urine by Head-Space Solid Phase Microextraction Followed by Gas Chromatography-Mass Spectrometry,” Journal of Chromatography B, Vol. 796, No. 1, 2003, pp.55-62.
[27] J. N. Miller and J. C. Miller, “Statistics and Chemometrics for Analytical Chemistry,” 4th Edition, Prentice-Hall, Harlow, 2000.
[28] L. H. Keith, “Compilation of EPA’s Sampling and Analysis Methods,” 2nd Edition, CRC Press, Boca Raton, 1996. http://dx.doi.org/10.1201/9781420050615

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