• Bulletin of the Korean Chemical Society
• /
• v.34 no.1
• /
• pp.139-142
• /
• 2013

A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

• Journal of Food Hygiene and Safety
• /
• v.14 no.1
• /
• pp.76-83
• /
• 1999

Solid phase microextraction (SPME) was used for the determination of 6 standard solvents (methanol, isopropanol, methyl ethyl ketone, ethyl acetate, cyclohexane, toluene) in food packaging materials. SPME method is a solvent-free sample preparation technique in which a fused silica fiber coated with polymeric organic liquid is introduced into the headspace above the sample. SPME method using fiber coated polydimethylisiloxane (PDMS) was compared with static headspace (SHS) method used as a reference. It was found that the optimal adsorption condition using PDMS-SPME method was 2$0^{\circ}C$ for 15 minutes for the standard solvents. Detection limits, linearity, reproducibility and recovery of both SHS and PDMS-SPME methods have been determined using 6 standard solvents. Both methods were characterized by high reproducibility and good linearity. Using SHS methods, the mean recovery of the 6 standard solvents was ranged from 75.5% to 105.8% with a mean relative standard deviation (RSD) of 0.3% to 4.8%. With PDMS-SPME method, the mean recovery of the 6 standard solvents was ranged from 86.7% to 108.3% with a mean RSD of 0.4% to 2.5%. The detection limits of both methods were the same for toluene, cyclohexane and methyl ethyl ketone; those of PDMS-SPME method were higher than those of SHS method for methanol, isopropanol and ethyl acetate. PDMS-SPME fiber shoed excellent adsorption for non-polar solvents such as toluene, while it showed relatively low adsorption for polar solvents such as methanol.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.31 no.1
• /
• pp.26-31
• /
• 2002

Volatile compounds from three parts of needles, sprouts and twigs in Pinus densiflora were extracted by solid phase microextraction (SPME) and dynamic headspace analysis (DHA). separated by gas chromatography, and identified by using mass selective detecter and Kovat's retention index. The amounts of monoterpenes isolated by SPME and DHA were 66.7% and 14.3% in needles, 90.6% and 0.7% in sprouts, and 90.6% and 1.2% in twings, respectively. The amounts of sesquiterpenes detected only by SPME were 25.8% in needles, 4.4% in twings and 1.5% in sprouts. And the amounts of oxygenated terpenes isolated by SPME and DHA were 4.7% and 79.0% in sprouts, 3.7% and 70.4% in twigs, and 1.0% and 50.7% in needles, respectively. The kinds of volatile compounds isolated by SPME were similar to those by solvent extraction, but the number of compounds identified to hate a boiling point below 5$0^{\circ}C$ by UHA was larger than that of SPME.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
• /
• 2001.09a
• /
• pp.148-150
• /
• 2001

Solid-phase microextraction (SPME) was investigated to understand the BTEX extraction behavior of SPME in groundwater. Analytical procedure was conducted In both conventional and headspace mode. And the conventional direct extraction method and the headspace analysis method were compared. Data obtained with direct and headspace SPME were very similar and showed successful results. In headspace analysis, the linearity was better and RSD (relative standard deviation, %) was smaller than direct extraction.

• Analytical Science and Technology
• /
• v.13 no.3
• /
• pp.277-281
• /
• 2000

The solid phase microextrction (SPME) fiber which contains $100{\mu}m$ polydimethyl siloxane of a stationary phase was used for the analysis of volatile organic compounds contained in aqueous solution. sixteen volatile organic compounds, which were spiked in blank water and extracted by the headspace SPME techique, were analyzed by gas chromatography/mass spectrometry (GC/MS). Analytical results showed that the percent of average recoveries and relative standard deviations were 97% and 4.7%, respectively. The value of detection limit was ranged from 0.01 to $0.5{\mu}g/l$. These results are more accurate than those obtained by the other methods such as purge and trap and headspace methods.

• Journal of Korean Society for Atmospheric Environment
• /
• v.24 no.3
• /
• pp.357-366
• /
• 2008

In this study, the analytical performance of trimethylamine (TMA) were investigated with respect to headspace-solid phase microextraction (HS-SPME) method. In order to induce the elution of aqueous TMA to headspace, NaOH was added as a decomposition reagent to aqueous TMA standard. By controlling the combination of three major variables for TMA extraction, the extent of extraction was compared between the two contrasting conditions for each variable (i.e., reaction time (long (L) vs short (S)), exposure temperature (30 vs $50^{\circ}C$), and exposure time (10 vs 30 min)). The results of this comparative analysis showed that the extraction efficiency for all eight types of HS-SPME combinations decreased on the order: L-30-30>L-50-10>L-30-10>L-50-30>S-30-30>S-50-30>S-50-10>S-30-10. The effect of reaction time appeared to exert significant influences on the relative recovery rate of HS-SPME at 90% confidence level. However, the effects of exposure temperature or exposure time were not so significant as reaction time. When the recovery rate of HS-SPME is compared against the direct injection of liquid standard into GC injector, it recorded as 2%. According to this comparative study, the reaction conditions for HS-SPME application can exert significant influences on the analysis of TMA.

• Korean Journal of Medicinal Crop Science
• /
• v.10 no.2
• /
• pp.120-125
• /
• 2002

This study was carried out to find the possibility of use of Solid Phase Microextraction (SPME) for extracting the volatile aroma compounds in the five aromatic plants (Agastache rugosa O. Kuntze, Mentha arvensis Linne, Thymus quinquecostatus Celakovsky, Elsholtzia splendens Nakai, Schizonepta tenuifolia Briquet) belongs to the Labiatae. In the result of the analysis, the volatile aroma compounds were mainly composed monoterpene alcohol (linanol, menthol, ${\alpha}-terpineol$, borneol), monoterpene ketone (limonene, menthone) and sesquiterpene (trans-caryophyllene,${\delta}-cadinene)$. The volatile aroma compounds of Agastache rugosa O. Kuntze and Mentha arvensis Linne were extracted by SPME more identified than the SDE. However, Schizonepta tenuifolia Briquet more identified by the SDE and in Elsholtzia splendens Nakai similar to the SDE. Especially, the SPME showed the sesquiterpene contents was more than the SDE. The major volatile aroma compounds were difference but the composition of those between the SPME and the SDE showed no difference. Within the results, the SPME showed the most convenient and a rapid extraction method to analysis of the volatile aroma compounds.

• The Korean Journal of Food And Nutrition
• /
• v.16 no.4
• /
• pp.372-378
• /
• 2003

The volatile components of cinnamon bark were extracted by using different isolation methods, simultaneous distillation extraction (SDE) and solid phase microextraction (SPME). Then the volatile components were analyzed by gas chromatography(GC) and mass selective detector(MSD). 30 compounds were identified in cinnamon bark. In SPME technique, several factors influencing the equilibrium of the aroma compounds between sample and SPME fiber was taken into account, including the kind of SPME fiber, extraction temperature and extraction time. Four different SPME fibers were tested, namely polydimethylsiloxane (PDMS), poly acrylate(PA), divinyl- benzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS) and carbowax/divinylbenzene(CW/DVB). Among these SPME fiber, PDMS coating fiber showed the best results. The profile of volatile compounds of cinnamon bark at different extraction temperature and extraction time were investigated by 100$\mu\textrm{m}$ PDMS fiber.

• Korean Journal of Food Science and Technology
• /
• v.33 no.1
• /
• pp.153-156
• /
• 2001

Traditional static headspace and headspace solid-phase microextraction(SPME) techniques were compared for their effectiveness in the extraction of volatile flavor compounds from the headspace of persimmon vinegar. The adsorption condition of SPME fiber for equilibrated headspace vapor was selected as $80^{\circ}C$ and 20 min. Total FID response for volatiles of persimmon vinegar was exactly higher such as total peak area $18.18{\times}10^6$ in SPMEGC technique than total peak area $1.35{\times}10^6$ in static headspace-GC. The major volatiles in persimmon vinegar were acetic acid, ethyl acetate, 3-hydroxy-2-butanone, ethanol, phenethyl alcohol. From static headspace-GC technique, 3 acids, 3 aldehydes, 5 alcohols, 9 esters and 1 ketone were identified. From SPME-GC technique, total 34 compounds including 6 acids, 7 aldehydes, 6 alcohols, 9 esters, 2 hydrocarbones, 1 ketone, 3 others were detected. Also the ratio for benzaldehyde, phenethylacetate and phenethylalcohol were higher in SPME-GC.

• Journal of Environmental Science International
• /
• v.19 no.12
• /
• pp.1447-1454
• /
• 2010

In this study, the detection limits of lower fatty acids in air were investigated by using Dynamic SPME(Solid Phase Micro-Extraction), i.e. improved Head Space - SPME method(HS-SPME). This Dynamic SPME, called SPDE(Solid Phase Dynamic Extraction), is the analytical method for volatile compounds in air with the extraction by using a stainless steel needle of which inner surface is coated with adsorption material and following the gas chromatographic analysis by inserting the needle into a injection port of GC and subsequently, desorption of the volatile compounds into a gas-chromatographic column. Extraction was carried out by passing the sample air through the needle with a suction pump which has been used for a detection tube. The result of measurement for the 6 lower fatty acids showed that the detection limits ranged from 0.10 ppm to 0.44 ppm and the linear correlation coefficients were over 0.99. Relative standard deviations obtained from 5 analytical repetition of a ca. 1.6 ppm standard mixture were in the range of 1.87%~2.47%. This method has been shown to be a adequate for the measuring C2~C5 fatty acids in air in the concentrations of over several hundreds ppb.