• Mass Spectrometry Letters
• /
• v.4 no.1
• /
• pp.18-20
• /
• 2013

Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

• Analytical Science and Technology
• /
• v.16 no.6
• /
• pp.458-465
• /
• 2003

The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.

• Applied Biological Chemistry
• /
• v.37 no.2
• /
• pp.115-123
• /
• 1994

Allelopathic activity of the volatiles from leaves of Perilla frutescens an Artemisia asiatica was determined on the basis of bioassay, which tested germination and seedling growth of radish, rice, mung bean and lettuce. Seedling growth was more inhibited by phytotoxic volatiles than germination. Volatile components collected by headspace cold trapping-Tenax GC adsorption were analyzed by GC-MS. Fifteen volatile components in P. frutescens and 15 components in A. asiatica were identified. By steam distillation-extraction, 4 flavor components in P. frutescens and 10 components in A. asiatica were identified. The inhibitory activity of the fractions, obtained by steam distillation-extraction, was determined by virtue of bioassay on radish. Volatile allelochemicals of the most active fraction, neutral fraction, isolated from P. frutescens contained 9 components. In A. asiatica, 24 volatile allelochemicals were identified.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
• /
• 2003.09a
• /
• pp.458-461
• /
• 2003

Solid-phase microextraction (SPME) and gas chromatography/headspace techniques(HS) and flame ionization detection (GC/FID) have been combined for determination of very polar compounds in water, including the widely used gasoline oxygenates and by-products. A relatively simple extraction method using a CAR/PDMS(75${\mu}{\textrm}{m}$) SPME fiber was optimized for the routine analysis of gasoline oxygenates and by-products in groundwater and reagent water. A sodium chloride concentration of 25%(w/w) combined with an extraction time of 20 min provided the greatest sensitivity while maintaining analytical efficiency Replicate analyses in fortified reagent and groundwater spiked with microgram per liter concentrations of gasoline oxygenates and by-products indicate quantitative and reproducible recovery of these and related oxygenate compounds. Method dynamic range was 50$\mu\textrm{g}$ L-1 to 3000$\mu\textrm{g}$ L-1 for gasoline oxygenates and by-products.

• Analytical Science and Technology
• /
• v.24 no.6
• /
• pp.421-428
• /
• 2011

In this study, headspace disk type monolithic material sorptive extraction (HS-MMSE) was developed, validated and applied to the analysis of volatile aroma compounds from vanilla perfume by gas chromatography -mass spectrometry (GC/MS). HS-MMSE uses monolithic material (MonoTrap) based on silica bonded with octadecyl silane (ODS) and activated carbon as a sorbent. Aroma compounds was adsorbed onto the MonoTrap in headspace and extracted by only 100 ${\mu}L$ of solvent. Total 12 volatile compounds from vanilla perfume were successfully analyzed using HS-MMSE. The influence of extractive parameters was investigated and optimized, using benzyl acetate, linalyl acetate, vanillin, ethyl vanillin as target compounds. Under the optimum condition, the limit of detection (S/N = 3) and the limit of quantification (S/N = 10) of proposed method for the target compounds were obtained within the range of 8.35~13.76 ng and 27.82~45.88 ng, respectively. The method showed good linearity with correlation coefficient more than 0.9888, satisfactory recovery and reproducibility. These results showed that HS-MMSE using disk type MonoTrap is a new promising technique for the analysis of volatile aroma compounds from vanilla perfume.

• Applied Biological Chemistry
• /
• v.51 no.3
• /
• pp.233-237
• /
• 2008

The essential oil was obtained from the aerial part of Rhododendon mucronulatum Turcz. var. ciliatum Nakai by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the oil were analyzed by gas chromatography-mass spectrometry (GC-MS). Nineteen constituents were identified from the essential oil: 15 carbohydrates, 3 alcohols, and 1 acetates. Major constituents were 2-${\beta}$-pinene (16.1%), camphene (11.9%), ${\delta}$-3-carene (11.4%), d,l-limonene (9.5%), and ${\gamma}$-terpinene (9.5%). By SPME extraction, seventeen constituents were identified: 13 hydrocarbons, 1 alcohol, 1 nitrogen-containing compound, 1 acetate, and 1 amine. Major constituents of the SPME-extracted sample were cam phene (19.6%), 2-${\beta}$-pinene (18.0%), ${\delta}$-3-carene (17.4%), trimethyl hydrazine (9.7%), ${\gamma}$-terpinene (8.5%), and d,l-limonene (5.5%). By HS extraction, thirteen constituents were identified: 11 hydrocarbons, 1 alcohol, and 1 nitrogen-containing compound. Major constituents of the HS-extracted sample were camphene (25.8%), ${\delta}$-3-carene (24.8%), 2-${\beta}$-pinene (20.2%), d,l-limonene (5.4%), tricyclene (5.1%) and trimethyl hydrazine (4.6%). The fragrance of the essential oil was coniferous, balsamic, and woody, and the $IC_{50}$ value of the essential oil was 0.030 ${\mu}g/mg$ in MTT assay using UaCaT keratinocyte cell line.

• Analytical Science and Technology
• /
• v.25 no.1
• /
• pp.39-49
• /
• 2012

A method to detect 37 volatile organic compounds (VOCs) in surface water was described based on headspace solid-phase micro extraction and gas chromatography-mass spectrometry. VOCs in water were vaporized for 30 min at 40 $^{\circ}C$ in a headspace vial and adsorbed on 85 ${\mu}m$ carboxen-polydimethylsiloxane. Under the established condition, the lowest quantification limit was 4.1-96 ng/L by using 4.0 mL water sample, and the relative standard deviation was less than 15% at concentrations of 0.05 and 0.50 ${\mu}g/L$. The detection limits meet lower concentration than 1/10 of the water quality criteria for VOCs established by the US EPA or Germany. The LOQ is a sensitivity which the monitoring for the establishing water quality criteria requires. When the proposed method was used to analyze the target compounds in sixteen surface water samples and total 16 VOCs were detected in surface water samples collected from Gum-River. Maximum concentrations of VOCs detected were not exceeded the EPA or Germany guidelines in any of the samples.

• Analytical Science and Technology
• /
• v.33 no.2
• /
• pp.76-85
• /
• 2020

A stainless-steel needle (Hamilton 90022, 22 gauge, 718-㎛ o.d., 413-㎛ i.d., 51-mm length, bevel tip) with an electrochemically coated polyaniline layer having a microbore tunnel was newly prepared as a device for headspace in-needle microextraction. For designing the needle, the polyaniline layer length was optimized, and to evaluate the extraction efficiency for polycyclic aromatic hydrocarbons, numerous cyclic voltammetry scans were conducted. In addition, the optimization of the analytical conditions (including the adsorption and desorption parameters) and the validation of the analytical method were conducted. The optimized adsorption and desorption conditions were 40 ℃ for 30 min and 230 ℃ for 60 s, respectively. Finally, in this study, a polyaniline layer was electrochemically deposited on the in-needle surface, and it exhibited good thermal stability. The needle with the polyaniline layer was repeatedly used more than 200 times during this study. This method has some advantages in terms of the extraction time, extraction efficiency, and analysis cost.

• Bulletin of the Korean Chemical Society
• /
• v.35 no.1
• /
• pp.211-217
• /
• 2014

A new needle-based device for headspace wire coated in-needle microextraction (HS-WC-INME) was fabricated using a nichrome wire coated with poly(ethylene glycol) (PEG) and poly(dimethylsiloxane) (PDMS) mixture. The proposed needle device was applied for the determination of volatile compounds in lavender and lavandin essential oils by gas chromatography. Fundamental parameters such as needle design, conditions of extraction and desorption were optimized along with the validation of the extraction and desorption efficiency. The optimal conditions were 30 min extraction at $50^{\circ}C$ and 2 min desorption at $240^{\circ}C$. The calibration curves showed good linearity with the suitable values of the coefficients of determination ($r^2$) greater than 0.99. The limits of detection for linalyl acetate, ${\beta}$-caryophyllene, linalool and (+)-limonene were 7.15, 9.04, 10.79 and 22.26 ng, respectively. Analytical recoveries were acceptable in the test samples, varying from 86.7% to 108.0%. The values of relative standard deviations for run to run showed range less than 0.9% while 3.9% through 7.2% for needle to needle. The proposed PEG-PDMS coating could be more suitable than PDMS coating to extract particular polar groups such as alcohols.

• KSBB Journal
• /
• v.23 no.3
• /
• pp.193-198
• /
• 2008

In this study, the supercritical $CO_2$ extraction was applied for the enrichment of coffee flavors. The extraction efficiency of coffee flavors was dependent on the pressure and temperature and optimized as 350 bar and 80$^\circ$C. Five flavors of high aroma values were analyzed. The flavors extracted by the supercritical $CO_2$ extraction were 76.6 times higher than those by the traditional method, espresso extraction. The modified headspace system proved the enhanced efficiency of supercritical $CO_2$ extraction. The coffee beverage containing the extract of supercritical $CO_2$ resulted 2.3 times of flavor enrichment when it was compared to that without the supercritical extract.