Evaluation of the Efficiency of Solvent Systems to Remove Acetic Acid Derived from Pre-pulping Extraction

Seong Jik Park,Joon Kwan Moon,Byung Hwan Um 한국목재공학회 2013 목재공학 Vol.41 No.5

Hemicellulose extract obtained by pre-pulping extraction of woodchips, is very diluted acidic in nature. The major component responsible for this weak acidity is acetic acid, present in levels up to 5~10 g/L. Here, we report an exploratory study on the extract upgrading by reactive solvent extraction of acetic acid as well as ASPEN simulation. In this study, liquid-liquid equilibria for the ternary systems (water + acetic acid + ethyl acetate) were measured at the temperature of 298.15 K and 10 (pH = 2.02), 5 (pH = 2.17), and 1 (pH = 2.48) percent of acetic acid samples were used to carry out liquid-liquid extraction studies using ethyl acetate. In a one-stage batch experiment, 96.0% of acetic acid could be extracted for the solvent when the ratio of organic-to-aqueous phases is 4:1. For simulation results, they were used to estimate the interaction parameters between each of the three compounds of the systems studied for the NRTL and UNIQUAC models. The estimated interaction parameters were successfully used to predict the equilibrium compositions by the two models.

Cross-examination of liquid-liquid extraction (LLE) and solid-phase microextraction (SPME) methods for impurity profiling of methamphetamine

Lee, J.,Park, Y.,Yang, W.,Chung, H.,Choi, W.,Inoue, H.,Kuwayama, K.,Park, J. Elsevier Sequoia 2012 Forensic Science International Vol. No.

Impurities in 48 methamphetamine (MA) samples were analyzed by liquid-liquid extraction (LLE) and headspace solid-phase microextraction (HS-SPME) methods. MPS-2 autosampler was used to improve reproducibility of SPME method, and nonadecane (C<SUB>19</SUB>) diluted with potassium bromide (KBr) powder was used as an internal standard for standardizing retention time. Impurities identified by SPME method showed different patterns compared with LLE method. Non-volatile impurities like methamphetamine dimer were not identified by SPME method, but some volatile impurities like diphenylketone, caprolactam and lots of unknowns were identified only by SPME method. 1-Phenyl-2-propanone (P2P), 1-phenyl-2-propanol and benzylcyanide peaks could be discriminated clearly by SPME method without interference of amphetamine, an artifact originates from MA degradation. Differences in the impurity patterns resulted in different clustering results. When 48 MA samples were classified into 5 LLE and 5 SPME clusters, cross-matching of the clusters resulted in 8 sub-clusters. It shows that combination of the different extraction methods can distinguish the differences which cannot be distinguished by LLE or SPME method alone, and can improve reliability of the profiling results.

Comparative Study of Extracting Fragrance Allergens by GC-MS/MS

( In Ja Lee ),( Jae-chan Ahn ),( Bogsoon Kim ),( Deukmo Chung ) 한국질량분석학회 2017 Mass spectrometry letters Vol.8 No.1

Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low logK_OW values (below about 2.5) were not extracted, and the correlation coefficient (r²) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were 0.078 ~ 0.582 μg/L and 0.261 ~ 1.940 μg/L, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient (r²) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were 0.020 ~ 0.138 μg/L and 0.065 ~ 0.440 μg/L, respectively.

Comparative Study of Extracting Fragrance Allergens by GC-MS/MS

Lee, In Ja,Ahn, Jae-Chan,Kim, Bogsoon,Chung, Deukmo Korean Society for Mass Spectrometry 2017 Mass spectrometry letters Vol.2 No.1

Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low $logK_{OW}$ values (below about 2.5) were not extracted, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were $0.078{\sim}0.582{\mu}g/L$ and $0.261{\sim}1.940{\mu}g/L$, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were $0.020{\sim}0.138{\mu}g/L$ and $0.065{\sim}0.440{\mu}g/L$, respectively.

Comparative Study of Extracting Fragrance Allergens by GC-MS/MS

이인자,안재찬,김복순,정득모 사단법인 한국질량분석학회 2017 Mass spectrometry letters Vol.8 No.1

Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low logKOW values (below about 2.5) were not extracted, and the correlation coefficient (r²) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were 0.078 ~ 0.582 μg/L and 0.261 ~ 1.940 μg/L, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient (r²) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were 0.020 ~ 0.138 μg/L and 0.065 ~ 0.440 μg/L, respectively.

어류에서의 과불화합물 분석을 위한 전처리법 확립 및 모니터링

허진주(Jin Ju Heo),이지우(Ji Woo Lee),김승규(Seung Kyu Kim),오정은(Jeong Eun Oh) 大韓環境工學會 2013 대한환경공학회지 Vol.35 No.7

본 연구에서는 어류에서 16종의 과불화합물을 분석하기 위한 최적 전처리법을 확립하고자 이온쌍 추출법(IPE)과, 액-액 추출법(LLE), 고체상 추출법(SPE), 이온쌍 + 고체상 추출법(IPE + SPE) 각각에 대하여 내부표준물질의 주입 시기를 달리하여 회수율을 비교하였다. 내부표준물질을 추출 전에 주입하는 IPE-before법이 가장 효율적인 전처리법으로 평가되었다. 추가로 RPM 및 pH 테스트를 통해 IPE-before법을 적용한 분석 전처리 효율을 더 개선할 수 있었다. 확립된 전처리법을 이용해 국내마트에서 구입한 33개의 어류 및 어류의 간과 내장시료에서 과불화합물을 분석하였다. 16종 과불화합물의 검출범위는 ND~1.67ng/g이었으며, 검출빈도는 100%로 나타났다. 어류의 근육부와 간, 내장을 비교 모니터링 한 결과, 간(17.8 ng/g) > 내장(13.3 ng/g) >근육부(1.67 ng/g) 순으로 과불화합물이 검출됨을 확인하였다. 국외 선행연구 결과와 비교하였을 때, 본 연구에서의 어류의 농도는 비슷하거나 낮게 검출되었다. An efficient extraction method was developed for the analysis of 16 perfluorinated compounds (PFCs) in fish samples. We compared the recoveries from the Ion-Pairing Extraction (IPE), Liquid-Liquid Extraction (LLE), Solid-Phase Extraction (SPE), IPE + SPE method with varying the injection time of the internal standard. As a result, IPE method with the internal standard before extraction was evaluated as the most effective pretreatment method. The RPM (Revolution Per Munite) and pH in IPE-before method were additionally adjusted and the more efficient pretreatment method was established. The total 33 fish samples including liver and gut samples were collected from Korean markets and analyzed PFCs with developed pretreatment method of this study. Total 16 PFC levels in fish samples ranged from ND to 1.67 ng/g with 100% detection frequency. The average PFCs concentrations of muscle, liver and gut samples from fish were compared and showed the following trend: liver (17.8 ng/g) > gut (13.3 ng/g) > muscle (1.67 ng/g). The PFC levels in fish samples were similar or lower than other available previous results of foreign studies.

LC-MS/MS를 이용한 넙치(Paralichthys olivaceus)시료의 톨트라주릴 및 톨트라주릴 설폰 분석

홍도희,김아현,이가정,윤민철,손광태,김명석,김나영,정승희,조미라 한국수산과학회 2019 한국수산과학회지 Vol.52 No.5

Several studies investigating the prevention and treatment of external parasites in farmed olive flounder Paralichthys olivaceus have found that the anticoccidial agent toltrazuril sulfone is an effective antiparasitic. Prior to undertaking a full-scale study, we developed analytical methods to detect the levels of toltrazuril and toltrazuril sulfone in farmed flounder samples using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-MS/MS). This analysis showed that LC-MS/MS changed the mobile phase and collision energy of toltrazuril and toltrazuril sulfone. This was validated using established conditions. Sample pre-treatment for this process involved extraction with dichloromethane and purification by liquid–liquid extraction in formic acid, acetonitrile, and h-hexane, followed by determination of all compounds by LC-MS/MS. Separation was achieved within 10 min by gradient elution using a Capcell Pak C18 (3.0 μm, 100×2.0 mm) analytical column (Shiseido UG 120V) with a mixture of 0.1% (v/v) formic acid and acetonitrile. Multiple reaction monitoring was used for selective detection of toltrazuril and toltrazuril sulfone. This method yields satisfactory results for linearity, precision, and limits of quantification. Therefore, the method established in our study will serve as a basis for further research on parasite control by toltrazuril and toltrazuril sulfone.

The Optimization of Value Added Chemicals Recovery by Liquid to Liquid Extraction for Black liquor Derived from Kraft Pulping

HeeSun KWON,YongSeon KIM,SeJin KIM,SunHeon CHOI,ByungHwan UM 한국생물공학회 2014 한국생물공학회 학술대회 Vol.2014 No.10

Geosmin과 2-MIB의 GC/MS 분석을 위한 전처리 방법 비교 연구

임형인,배주순,이소영,김민영,장성국,김지우,남지현,이덕안 한국환경기술학회 2022 한국환경기술학회지 Vol.23 No.3

Geosmin and 2-methylisoborneol are representative odorous compounds that smells like mud or mold after rain, and are secondary metabolites generated by various organisms such as blue-green algae and actinomycetes. These substances, which are detected in raw water and purified water, are odor substances that have not been found to be harmful to the human, but induce an unpleasant taste and odor in tap water and cause distrust in drinking. Therefore, research on the cause and removal methods is continued, and a sensitive and accurate detection method is required. In this study, three pretreatment methods(LLE, SPE, HS-SPME) and SPME arrow were compared for the detection of Geosmin and 2-MIB. In the four methods, the limits of quantitation were 0.2-0.8 ng/L for Geosmin and 0.6-1.1 ng/L for 2-MIB. The accuracy and precision of all four methods met the target values for quality control, but the HS-SPME and the SPME Arrow showed the most satisfied results.

Simultaneous Determination of Sulfonamides in Porcine and Chicken Muscle Using High Performance Liquid Chromatography with Ultraviolet Detector

Yousin Shim,Dongbin Shin,Yongsun Cho,Yunhee Choi,Sanghee Lee 한국식품과학회 2009 Food Science and Biotechnology Vol.18 No.6

The present study used the liquid extraction pretreatment method and developed a liquid chromatographyultraviolet detector (LC-UV) for the simultaneous determination of 14 sulfonamides (SAs) residues in porcine and chicken muscle. Linearity within a range of 50-150 ㎍/㎏ was obtained with the correlation coefficient (r²) of 0.9673-0.9997. The mean recovery of SAs was 55.9-109.7% (relative standard deviations; RSDs 1.7-17.3%) in porcine muscle and 52.8-112.4% (RSDs 2.3-16.9%) in chicken muscle. The limits of detection (LODs) and limits of quantification (LOQs) were 2-32 and 7-96 ㎍/㎏ in porcine muscle, and 4-32 and 13-97 ㎍/㎏ in chicken muscle, respectively. These values were lower than the maximum residue limits (MRLs) established by the European Union. The sum of all SAs residues present should be less than 100 ㎍/㎏.