• Title/Summary/Keyword: Soxhlet

Search Result 171, Processing Time 0.217 seconds

Study on simultaneous determination of aromatic material causing allergic in children's products by GC-MSD (GC-MSD를 이용한 어린이 제품 중 알러지 유발 방향성 물질의 동시분석법 연구)

  • Ko, Kyeong Mok;Rhu, Chan Joo;Ko, Byeong Rae;Lee, Seok Ki
    • Analytical Science and Technology
    • /
    • v.33 no.3
    • /
    • pp.134-142
    • /
    • 2020
  • Twenty-one allergy-induced aromatic material in children's products were analyzed using gas chromatography mass spectrometer(GC-MSD). The analytes were extracted using an automatic Soxhlet extractor, centrifuged for 10 minutes in a fast freezing centrifuge, and the supernatant was filtered with a syringe filter and then transferred into a 2 mL vial and injected in a split mode. In the established condition, the calibration curve showed linearity with a determination coefficient of 0.9981 or more. Sensitivity was 0.3145 ~ 1.6757, which showed a fairly wide range of sensitivity for each substance. The detection limit of the device was 0.0016 ~ 0.0423 ㎍/mL and the maximum detection limit was less than 0.05 ㎍/mL. The method detection limit ranged from 0.0030 ~ 0.0589 ㎍/mL. In addition, the limit of quantification ranged from 0.0096 to 0.1876 ㎍/mL, with precision ranging from 0.41 to 10.49 % and accuracy ranging from 83 to 116 %. The analytical method developed in this study was applied to commercial products.

Characteristics and Sampling of Dioxins/Furans from Emission Gas and Fly Ash Produced in Municipal Waste Incinerator (도시 소각로 쓰레기 소각후 생성된 폐가스 및 비산재중에 포함된 다이옥신류의 측정 및 특성고찰)

  • Lim, Chae-Hyun;Kim, Hee-Taik;Sohn, Jung-Hyun;Chang, Yoon-Seok
    • Applied Chemistry for Engineering
    • /
    • v.8 no.5
    • /
    • pp.790-795
    • /
    • 1997
  • Polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofuransfurans are the archetype of toxic chemicals. So it has absorbed public attention. The majors primary sources of PCDDS and PCDFs are chemical, thermal and photochemical reactions. Municipal solid waste incinerator facilities has been reported as the major contributors of dioxins to the environment. In this paper, Dioxins and furans were examined emission gas and fly ash produced during combustion in municipal solid waste incinerator. More effective method for sampling, extraction was described. The sample was extracted using a soxhlet method and purified using silicagel, alumina and carbon fibre HPLC to remove interfering compound. The extract was then analyzed by HRGC/HRMS. The result of this study showed recovery standard was good and the data resembled those of thermal processes. Total dioxins and furans were $1076.20pg/Nm^3$ and $1452.34pg/Nm^3$ respectively. The amount of highly chlorinated compound was more than that of lowly chlorinated compound. The 2,3,7,8-substituted TCDD was Just 0.34% of the total dioxins/furans amount.

  • PDF

Studies on Benzo(a)pyrene of the Suspended Particulate in Atmosphere of Seoul City (서울시(市) 대기중(大氣中) 유해(有害) 부유분진(浮遊粉塵) 성분(成分)에 관(關)한 조사연구(調査硏究) -부유분진중(浮遊粉塵中)의 Benzo(a)pyrene에 관(關)하여-)

  • Kwon, Sook-Pyo;Chung, Yong;Lim, Dong-Koo
    • Journal of Preventive Medicine and Public Health
    • /
    • v.11 no.1
    • /
    • pp.65-75
    • /
    • 1978
  • This study was carried out to investigate air pollution by total suspended particulate(T.S.P.), benzene soluble matter and benzo(a) pyrene in Seoul city. The sampling areas were divided into commercial(Kwang Hwa Moon), indus-trial(Ku Ro Dong) and residensial area(Shin Chon). Sampling was undertaken by High Voulme Air Sampler for four seasons from January 1917 to November 1977. The T.S.P. was extracted with Soxhlet apparatus by benzene and benzo(a) pyrene was separated by column chromatography and thin layer chromatography. The concentrations of benzo(a) pyrene were measured by means of fluorophotometer, and following results were obtained. 1. Arithmetic average concentration for 1-day averaging time of total suspended particulate were $275.6ug/m^3$ in Kwang Hwa Moon, $325.9ug/m^3$ in Ku Ro Dong and $193.0ug/m^3$ in Shin Chon. 2. The seasonal variance of total suspended parti-culate at Ku Ro Dong and Shin Chon were $102.7ug/m^3\;99.6ug/m^3$ respectively and at Kwang Hwa Moon $39.9ug/m^3$. And the concentration of autumn is higher than of that spring at Ku Ro Dong and at Shin Chon, but at Kwang Hwa Moon, the seasonal variance is very little. 3. The concentrations of 50% frequency from geometric mean for 1-day averaging time were $264ug/m^3,\;300ug/m^3\;and\;178ug/m^3$ at Kwang Hwa Moon, Ku Ro Dong and Shin Chon. And geometric standard deviation were 1.27, 1.38 and 1.41 respectively. 4. The concentrations of benzene soluble mater were $26.9ug/m^3$ at Kwang Hwa Moon, $22.7ug/m^3$ at Ku Ro Dong and $15.5ug/m^3$ at Shin Chon, and the ratios to the T.S.P. were 9.8%(range 5.6-14.8%), 7.0%(range 2.4-14.4%) and 8.0%(range 5.5-22.1%) respectively. 5. The concentrations of benzo(a) pyrene were $8.5ug/m^3$ (range $0.8-29.9ug/m^3$) at Kwang Hwa Moon $10.9ug/m^3$(range $1.1-52.0ug/m^3$) at Ku Ro Dong and $5.8ug/m^3$(range $1.5-11.4ug/m^3$) at Shin Chon. 6. The results of this investigation were relatively high in compared with the recommended standards of suspended particulate in air of U.S. Environmental Protection Agency and observed levels of benzo(a)-pyrene in U.S. city.

  • PDF

Development of Analytical Method of Polycyclic Aromatic Hydrocarbons Deposited on Tree Leaves by GC/MS (GC-MS 에 의한 나뭇잎에 침착된 다환방향족 탄화수소의 분석)

  • Chun, Man-Young;Lim, Ceoel-Soo;Kim, Tae-Wook
    • Korean Journal of Environmental Agriculture
    • /
    • v.18 no.2
    • /
    • pp.135-139
    • /
    • 1999
  • A new effective and economic method was developed, removing interferences such as chlorophyll and lipid from leaves with small amounts of reagents and solvents in order to analyse PAHs(Polycyclic Aromatic Hydrocarbons). The extract from a soxhlet containing $4{\sim}5g$ of leaves and 100ml of dichlormethane and refluxed for 20 hrs was concentrated and eluted with 60ml of a hexane:dichloromethane (1:1) mixture through a column of 9mm wide inner diameter and 130mm long, packed from the bottom with 2.5g of $Al_2O_3$, 1.5g of $SiO_2$and 2g of anhydrous $Na_2SO_4$. The eluent was concentrated and loaded on a GPC column of 20mm wide inner diameter and 280mm long, packed with 12g of Bio-beads. The column was washed with 37ml of the hexane:dichloromethane(1:1) mixture. Another 43ml of the mixture was eluted as a PAH fraction and collected. This eluent was concentrated under gentle nitrogen to $50{\mu}l$ and analysed using GC-MS. The recoveries, obtained by comparing with the amounts of the internal standards of deuterated PAHs were $43.3{\sim}107.5%$(RSD $2.2{\sim}9.5%$).

  • PDF

Studies on the Fatty Acid Composition of Amorpha-fruticosa Seeds (Amorpha-fruticosa종자(種子)의 지방산조성(脂肪酸組成)에 관한 연구(硏究))

  • Whang, Byung-Ho;Lee, Sang-Young
    • Korean Journal of Food Science and Technology
    • /
    • v.6 no.2
    • /
    • pp.86-90
    • /
    • 1974
  • Quantitative analysis of the fatty acids contained in Amorpha-fruticosa seeds was carried out by means of gas chromatography with F.I.D. The general components and chemical constants have been performed with A.O.A.C methods. The results are summarized as follow: 1. General components of Amorpha-fruticosa seeds come out to be 17.65% moisture, 21.02% crude protein, 12.04% crude lipid and 5.37% ash. 2. Extraction of crude lipids were performed by soxhlet extractor for 14 hour. Amounts of the crude lipids were extracted 80.25% in ether, 80.00% in methanol, 77.34% in benzene and 69.96% in hexane. 3. Chemical constants of Amorpha-fruticosa seed oil were saponification number 178.67, acid number 3.11 and iodine number 54.27. 4. The fatty acid components of Amorpha-fruticosa seeds were quantitatively determined by gas chromatography to give 78.73wt% linoleic, 5.8wt% oleic, 5.68wt% palmitic, 4.8wt% stearic and 3.40wt% linolenic acid in ether solvent and to give 77.86wt% linoleic, 7.77wt% palmitic, 5.84wt oleic and 4.97wt% stearic acid in methanol solvent. The peak of capric acid was not found. Myristic, arachidic and lauric acids were very small.

  • PDF

Studies on the Fatty Acid Composition of Duck Meat (오리고기의 지방산조성(脂肪酸組成)에 관(關)한 연구(硏究))

  • Nam, Hyun-Keun
    • Journal of Nutrition and Health
    • /
    • v.10 no.1
    • /
    • pp.34-37
    • /
    • 1977
  • Quantitative analysis of the fatty acids contained in Duck meat was carried out by the Gas Chromatography with Flame ionization Detector, The general components and chemical constants have been performed with A.O.A.C. methods. The results art summarized as follows : 1. General composition of Duck meat come out to be 64.87% moisture, 19.06% protein, 17.05% fat, and 1.02% ash. 2. It was investigated that extraction of lipids were performed by Soxhlet extractor for 12 hours. Amounts of lipids were extracted 79.57% in ethylether, 70.15% in chloroform, and 72.35% in n-hexane. 3. Chemical constants of lipids in Duck meat were obtained as follows : Saponification number 201.5, Acid number 5.01, Iodine number 50.1 and Carbonyl number 4.5 4. It was investigated that the fatty acid component were quantitatively determined by the gas chromatography : Linolenic acid 1.6%, Linoleic acid 19.9%, Oleic acid 45.9%, Stearic acid 3.1% Palmitic acid 17.2% and Myristic acid 0.12% in leg portion. Linolenic acid 1.7% Linoleic acid 17.2%, Oleic acid 51.2%, Stearic acid 3.3%, Palmitic acid 17.1% and Myristic acid 0.17% in breast portion. 5. Cholesterol of blood, breast and leg portion fat in Duck were obtained as follows : Total cholesterol 200 mg%, 260 mg% , and 400 mg% respectively; cholesterol ester 120mg%, 151 mg%, and 240mg% respectively.

  • PDF

PREDICTION OF PHYSICO-CHEMICAL AND TEXTURE CHARACTERISTICS OF BEEF BY NEAR INFRARED TRANSMITTANCE SPECTROSCOPY

  • Olivan, Mamen;Delaroza, Begona;Mocha, Mercedes;Martinez, Maria Jesus
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
    • /
    • 2001.06a
    • /
    • pp.1256-1256
    • /
    • 2001
  • The physico-chemical and texture characteristics of meat determine the nutritional, technological and sensory quality. However, the analysis of meat quality requires expensive, laborious and time consuming analytical methods. The objective of this study was to evaluate NIR spectroscopy using transmittance for determining the moisture, fat, protein and total pigment content, the water holding capacity (WHC) and the toughness of beef meat. A total of 318 spectra were recorded from ground beef samples by a Feed Analyzer 1265 of Infratec. The samples were obtained from the Longissimus muscle of the 10$^{th}$ rib of yearling bulls, ground with an electrical chopper, vacuum packaged, aged during 7 days and frozen at -24$^{\circ}C$ until the analyses were done. Moisture content was measured by oven drying at 10$0^{\circ}C$, fat content was determined by Soxhlet extraction and protein content was estimated from nitrogen content using the Kjeldahl analysis. The total pigment content was determined by the method of Hornsey and the WHC using the method of filter paper press. The instrumental evaluation of texture (maximum load WB, maximum stress MS and toughness) was conducted in an Instron equipment with a Warner-Bratzler shearing device. This analysis was performed on a chop of 3.5 cm obtained from the longissimus of the 8$^{th}$ rib, aged during 7 days, kept frozen at -24$^{\circ}C$ and cooked before the analysis. Near infrared spectra were recorded as log 1/T (T=transmittance) at 2 nm intervals from 850 to 1050 nm using a Feed Analyzer 1265 of Infratec. Calibrations were performed with the WinISI software (vs. 1.02) using the MPLS method. To examine the effect of scatter correction o. derivation of spectra on the calibration performance, calibrations were calculated with the crude spectra or pretreated with different mathematical treatments (inverse MSC, SNVD) and/or second derivative operation. For chemical composition, the use of the scatter corrections improved the calibration statistics, in terms of lower SECV and higher $r^2$. In most of the variables, the use of the 2$^{nd}$ derivative improved the predictions, mainly when combined with the SNVD treatment. However, for predicting the texture traits, the best estimation was obtained from the crude spectrum. These results showed that the equations obtained for predicting moisture, fat and total pigments were very accurate, with $r^2$ being higher that 0.9. However, the prediction of the texture traits (WB, MS, toughness) from ground meat was poor.

  • PDF

A Study on the Synthesis of Eugenolchitosan and Safrolechitosan (Eugenol과 safrole을 부가한 chitosan 유도체 합성)

  • Kim, Je-Jung;Jung, Byung-Ok;Chang, Pahn-Shick;Park, Dong-Ki
    • Korean Journal of Food Science and Technology
    • /
    • v.36 no.3
    • /
    • pp.398-402
    • /
    • 2004
  • Safrolechitosan (SaCs) and eugenolchitosan (EuCs) were synthesized and characterized to increase water solubility and functionality of chitosan. Product impurities were removed by Soxhlet apparatus using methanol to obtain final product with high purity. Using Ubbelohde viscometer, molecular weights of chitosan, EuCs, and SaCs were determined as $1.2{\times}10^{5}\;Da,\;7.8{\times}10^{5},\;and\;7.5{\times}10^{5}\;Da,\;respectively$. IR spectrum of SaCs revealed chemical shift of amide II band ($1,553cm^{-1}$) of chitosan grafted by safrole caused by generation of covalent bond between primary amino of chitosan and double bond of safrole. Due to graft reaction of safrole onto chitosan, vinyl bands ($1,611\;and\;1,442cm^{-1}$) of safrole disappeared. In graft reaction of eugenol onto chitosan, shift of amide II band ($1,553cm^{-1}$) and disappearance of vinyl band were observed. On $^{1}H-NMR$ spectrum of EuCs, $H_{2}C=CH-$ peak in eugenol (monomer) disappeared, whereas $-H_{2}C-CH_{2}-$ peak appeared. Above results indicate safrole and eugenol were successfully grafted onto chitosan.

Quantitation of Phthalate and Adipate in Natural Mineral Water and PET Container (먹는 샘물 및 PET 용기 중 Phthalate와 Adipate의 정량분석)

  • Shin, Ueon-Sang;Ahn, Hye-Sil;Shin, Ho-Sang
    • Analytical Science and Technology
    • /
    • v.15 no.5
    • /
    • pp.475-481
    • /
    • 2002
  • The determination of phthalates and adipate in natural mineral water and its container is described. Phthalates and adipate were extracted from natural mineral water by liquid-liquid extraction with methylene chloride, concentrated and then injected in GC-MS (SIM). Phthalates and adipate from 1) PET, cap, label and glue were extracted in Soxhlet with 50 mL of carbon tetrachloride, purified with silicagel and detected with GC-MS (SIM). Peak shapes and quantitation of phthalates and adipate were excellent, with linear calibration curves over a range of $0.1{\sim}10{\mu}g/L$ in water sample ($r^2$ > 0.996) and over a range of $1{\sim}1,000{\mu}g/Kg$ in solid samples ($r^2$>0.994). The detection limits of analytes were $0.002{\sim}0.010{\mu}g/L$ in water and $0.01{\sim}0.02{\mu}g/Kg$ in solid samples. Five kinds of natural mineral water samples, two PETs, two labels, two caps and two glues were quantified by the described procedure. As a results, the concentrations of total phthalates in natural mineral water ranged from ND ~ 1.2 ng/mL. Otherwise, the concentrations of total phthalate extracted from PET ranged from 0.55 ~ 1.2 mg/Kg. We found that the accurate determination of phthalte and adipate in natural mineral water and container must be considered blank correction and the removal of label and glue in PET sample.

Simultaneous determination of aromatic material causing allergic in children's products by Gas Chromatography (어린이 제품 중 가스 크로마토그래피를 이용한 알러지 유발 방향성 물질의 동시분석법)

  • Ko, Kyeong Mok;Rhu, Chan Joo;Kim, Jong Won;Lee, Seok Ki
    • Analytical Science and Technology
    • /
    • v.31 no.1
    • /
    • pp.23-30
    • /
    • 2018
  • Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.