• Title/Summary/Keyword: SPME fiber type

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Evaluation of Volatile Compounds Isolated from Pork Loin (Longissimus dorsi) as Affected by Fiber Type of Solid-phase Microextraction (SPME), Preheating and Storage Time

  • Park, Sung-Yong;Yoon, Young-Mo;Schilling, M. Wes;Chin, Koo-Bok
    • Food Science of Animal Resources
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    • v.29 no.5
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    • pp.579-589
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    • 2009
  • This study was conducted to investigate the effects of heating, fiber type used in solid-phase microextraction (SPME, two phase vs three phase) and storage time on the volatile compounds of porcine M. longissimus dorsi (LD). Volatile compounds were measured using a gas chromatography and mass spectrometry (GC/MS) with a quadrupole mass analyzer. Among the volatile compounds identified, aldehydes (49.33%), alcohols (24.63%) and ketones (9.85%) were higher in pre-heated loins ($100^{\circ}C$/30 min), whereas, alcohols (34.33%), hydrocarbons (22.84%) and ketones (16.88%) were higher in non-heated loins. Heating of loins induced the formation of various volatile compounds such as aldehydes (hexanal) and alcohols. The total contents of hydrocarbons, alcohols, and carboxylic acids were higher in two phase fibers, whereas those of esters tended to be higher in three-phase fibers (p<0.05). Most volatile compounds increased (p<0.05) with increased storage time. Thus, the analysis of volatile compounds were affected by the fiber type, while heating and refrigerated storage of pork M. longissimus dorsi increased the volatile compounds derived from lipid oxidation and amino acid catabolism, respectively.

Analysis of Agrochemical Residues in Tobacco Using Solid Phase Microextraction-Gas Chromatography with Different Mass Spectrometric Techniques

  • Lee, Jeong-Min;Jang, Gi-Chul;Kim, Hyo-Keun;Hwang, Geon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.2
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    • pp.117-124
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    • 2008
  • A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.

Optimization of Headspace Sampling Using Solid Phase Microextraction For Volatile Organic Acids in Different Tobacco Types

  • Lee, Jang-Mi;Lee, Jeong-Min;Son, Seong-Ae;Kwon, Young-Ju;Jang, Gi-Chui;Kim, Young-Ho
    • Journal of the Korean Society of Tobacco Science
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    • v.35 no.1
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    • pp.7-12
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    • 2013
  • A Solid-phase micro extraction(SPME) was evaluated as a tool for headspace sampling of tobacco samples. Several experimental parameters (sampling temperature, pH, and type of SPME fibers) were optimized to improve sampling efficiency in two aspects ; maximum adsorption and selective adsorption of volatile organic acids onto SPME fibers. Among four types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate), Car/PDMS (Carboxen/Polydimethylsiioxane) and PDMS/DVB(Polydimethylsiioxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency. A variety of tobacco samples such as flue cured, burley and oriental were used in this study. The effect of these parameters was often dominated by the physical and chemical nature (volatility, polarity) of target compounds. This method allowed us to make important improvements in selectivity and sensitivity. The Car/PDMS fiber was shown to be the most efficient at extracting the 10 selected volatile organic acids. The parameters were optimized: $80^{\circ}C$ adsorption temperature, 30 min of adsorption time, $240^{\circ}C$ desorption temperature, 1 min of adsorption time.

Development of an analytical method of organochlorine pesticides in human bloods using head space-solid phase microextraction coupled with gas chromatography/mass spectrometry (HS SPME-GC/MS를 이용한 혈액 중 유기염소계 농약의 분석법 개발)

  • Kang, Tae-Woo;Pyo, Hee-Soo;Hong, Jong-Ki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.259-271
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    • 2008
  • The analytical method of extracting compounds from human blood to examine accumulated organochlorine pesticides (OCPs) has been widely used the traditional liquid-liquid extraction (LLE) method and solid-phase extraction (SPE) method, yet these methods have certain limitations in purification and usafe of a large amount of sample. In order to overcome the se problems reside in these, solid-phase microextraction (SPME), known as a highly efficient extration method with less samples and relatively simple, was employed to collect 18 different kinds of OCPs in blood as extraction method in this study. To optimize extraction method, we examine various experimental SPME-parameters such as adsorption (fiber type, adsorption time, adsorption temperature, salting out effect), and desorption (desorption time, desorption temperature etc.). From the experimental results, the optimal conditions are as follows: fiber was polyacrylate with $85{\mu}m$, adsorption time was for 5 min, adsorption optimum temperature was at $280^{\circ}C$, and salting out effect was NaCl with 0.1 g. MDL, precision and accuracy was in the ranges of 0.05~0.20 ng/mL, 5.59~13.39%, respedively, and accuracy was -0.5% ~24.5% for all OCPs.

Comparison of the volatile flavor compounds in different tobacco types by different extraction methods (추출방법에 따른 잎담배 종류별 휘발성 향기성분 특성비교)

  • Lee, Jang-Mi;Lee, Jeong-Min;Lee, Chang-Gook;Bock, Jin-Young;Hwang, Keon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.32 no.2
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    • pp.77-87
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    • 2010
  • Traditional simultaneous distillation extraction(SDE) and solid-phase micro extraction(SPME) methods using GC/MS were compared for their effectiveness in the extraction of volatile flavor compounds from different tobacco leaves types(flue-cured, burley, oriental). The major volatile flavor compounds of flue-cured and burley tobacco were similar such as neophytadiene, solanone, megastigmatrienone isomers, ${\beta}$-damascenone and ${\beta}$-ionone. On the other hand, volatile flavor compounds such as norambreinolide, sclareolide were specifically identified in oriental tobacco. Each method was used to evaluate the responses of some analytes from real samples and standards in order to provide sensitivity comparisons between two techniques. Among three types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate) and PDMS/DVB (Polydimethylsiloxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency, PDMS/DVB fiber was selected for the extractions of the volatile flavor compounds due to its effectiveness. The qualitative analysis showed that the total amount of volatile flavor compounds in SDE method(130 species) was much more than that in SPME method(85 species). SPME method was more efficient for all the highly volatile compounds than SDE method, but on the other hand, low-volatile compounds such as fatty acids or high-molecular hydrocabons were detected in SDE method. SPME method based on a short-time sampling can be adjusted to favor a selected group compounds in tobacco. Furthermore this results could be used to estimate the aroma characteristics of cigarette blending by using a different type of tobacco with more effectiveness and convenience.

Analysis of Breath from Diabetic Patients Based on a One-chip-type Sensor Array

  • Yu, Joon-Boo;Jang, Byoung Kuk;Byun, Hyung-Gi
    • Journal of Sensor Science and Technology
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    • v.28 no.4
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    • pp.221-224
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    • 2019
  • Based on the results of studies on acetone excretion in diabetic patients, a one - chip sensors array was fabricated by combining acetone-selective sensor materials and volatile-organic-compound sensitive sensor materials. An electonic-nose was implemented using a sensor array and confirmed selectivity for five gases. In this system, the excretion of diabetic patients and controls was sampled with solid phase microextraction fiber and transferred to the sensor array. Although the control and diabetic patients were distinct, several samples failed. In the control group, the results of blood tests were normal, but patients were highly obese. In addition, the gas chromatography mass spectrometry results for the subjects revealed chemicals that are external factors.