• Korean Journal of Food Science and Technology
• /
• v.39 no.2
• /
• pp.114-121
• /
• 2007

The purpose of this study was to investigate 253 kinds of pesticide residues in 58 commercial dried agricultural products in Seoul. The determinations of the pesticide residues were performed using multiresidue methods and were carried out by a gas chromatography-nitrogen phosphorus detector (GC-NPD), an electron capture detector ($GC-{\mu}ECD$), a mass spectrometry detector (GC-MSD) and high performance liquid chromatography-ultraviolet detector (HPLC-UV), and a fluorescence detector (HPLC-FLD). The pesticide residue detection rate in the commercial dried agricultural products was 24.1% (14 of 58 samples). Twelve pesticide residues without maximum residue limits (MRLs) were detected. In the vegetable groups, the frequency of pesticide residues was found to be in the increasing order of dried fruiting vegetables > dried leafy vegetables > dried stalk and stem vegetables. The pesticides used on dried red pepper in the dried fruiting vegetables were varied (7 kinds) and numerous (4 of 8 samples). The pesticide types detected in the commercial dried agricultural products were in the order of pyrethroid > organochloride > organophosphorus and insecticide > fungicide > herbicide ${\cdot}$ nematicide. The primary pyrethroid pesticide detected was cypermethrin. According to the producing areas of products, large numbers of pesticide residues were found in the order of Korea, China, North Korea, USA, and Vietnam.

• Journal of Food Hygiene and Safety
• /
• v.32 no.4
• /
• pp.284-289
• /
• 2017

Oxidized polyethylene wax (OPEW) is, one of the food additives, used as a coating agent in citrus fruits and nuts. OPEW is authorized to quantum satis in EU, USA, and is acceptable less than 250 mg/kg in Australia and New Zealand. But OPEW is unauthorized as a food additive in Korea. This study was to establish the analytical method of OPEW and demonstrate the effective application of various food samples. We first conducted to compare the various analytical method including acid value (AV), high temperature gel permeation chromatography (HT-GPC), matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF/MS), gas chromatography flame ionization detector (GC-FID) and fourier transform infrared spectroscopy (FT-IR). This result indicated that FT-IR spectrum of OPEW treated food sample displayed absorption bands for carbonyl group (C=O, $1714cm^{-1}$), ester group (C-O, $1463cm^{-1}$), aliphatic group (C-H, $2916cm^{-1}$). Furthermore, IR spectrum of OPEW treated food sample showed similar tendency with IR spectrum of OPEW standard. Therefore, it is confirmed that analytical method using FT-IR can be detected on analysis of OPEW in food. As a result of monitoring of 111 samples using established analytical method, OPEW was not detected in the food samples.

• Korean Journal of Food Science and Technology
• /
• v.45 no.1
• /
• pp.20-24
• /
• 2013

Food irradiation has recently become one of the most successful techniques to preserve food with increased shelf life. This study aims to analyze hydrocarbons in almonds (Prunus amygosalus L.) and peanuts (Arachis hypogaea) induced by electron beam irradiation. The samples were irradiated at 0, 1, 3, 5 and 10 kGy by e-beam and using florisil column chromatography fat, and content was extracted. The induced hydrocarbons were identified using gas chromatography-mass spectrometry (GC/MS). The major hydrocarbons in both irradiated samples were 1,7-hexadecadiene ($C_{16:2}$) and 8-heptadecene ($C_{17:1}$) from oleic acid, 1,7,10-hexadecatriene ($C_{16:3}$) and 6,9-heptadecadiene ($C_{17:2}$) from linoleic acid and 1-tetradecene ($C_{14:1}$) and pentadecane ($C_{15:0}$) from palmitic acid. Concentrations of the hydrocarbons produced by e-beam were found to be depended upon the composition of fatty acid in both almonds and peanuts. The $C_{n-2}$ compound was found to be higher than $C_{n-1}$ compound in oleic acid and palmitic acid, while in case of linoleic acid, $C_{n-1}$compound was higher than $C_{n-2}$ compound. The radiation induced hydrocarbons were detected only in irradiated samples, with 1 kGy or above, and not in the non-irradiated ones. The production of 1,7-hexadecadiene ($C_{16:2}$), 8-heptadecene ($C_{17:1}$), 1,7,10-hexadecatriene ($C_{16:3}$) and 6,9-heptadecadiene ($C_{17:2}$), in high concentration gave enough information to suggest that these may be the possible marker compounds of electron beam irradiation in almonds and peanuts.

• Korean Journal of Food Science and Technology
• /
• v.45 no.5
• /
• pp.531-536
• /
• 2013

We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

• Clean Technology
• /
• v.17 no.2
• /
• pp.124-133
• /
• 2011

In addition to six substances regulated in EU RoHS including lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE), priority substances are identified in new RoHS II as hexabromocyclododecane (HBCDD), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP) and diethylhexyl phthalate (DEHP). In this study, 20 plastic samples were collected from 12 domestic electrotechnical companies and levels of four restricted substances were determined by gas chromatography-mass spectrometry, Among 20 parts that compose washer, refrigerator or microwave oven, HBCDD was detected in three samples of NBR material with the amount of 42~381 mg/kg while DBP and BBP was not detected in any samples collected respectively, implying that these substance may not be used widely in plastic materials for EEE. However, DEHP was detected in all samples of NBR, PP, PBT, EPDM and PVC materials with the amount of 42 up to 59,400 mg/kg that exceeds the limit value of 0.1 wt% (1,000 mg/kg). Presence of a restricted substance in polymer material makes a great negative influence on a number of final product. To cope with coming RoHS II as well as REACH, action not to use DEHP in plastic material or the relevant notification in case of REACH seems to be needed. Screening test of Arsenic compounds such as diarsenic pentaoxide, diarsenic trioxide, lead hydrogen arsenate, triethyl arsenate that are included in REACH SVHC was done by ICP measurement Arsenium was detected in four samples made of NBR and PBT materials in the level of 15~700 mg/kg. By considering the screening method used in this study, the amount of arsenium compounds in the thermistor made of PBT material has a high chance of exceeding the regulated limit value.

• Korean Journal of Environmental Agriculture
• /
• v.26 no.1
• /
• pp.62-68
• /
• 2007

Concerns about endocrine disrupting chemicals emitted from humans and animals have been increased because these compounds are detected at very low levels in environment and adversely affect on indigenous fauna. To date, there is little information regarding the concentration of these compounds in animal wastes. In this study, the female hormones, $17\beta-estradiol$ (E2), estrone (E1) and estriol, were measured to provide baseline data in animal wastes. Samples were collected from animal waste storage, methane digester and sludge separated wastewater and analyzed by gas chromatography-mass spectrometry. To measure the mass ratios of estrogen to macronutrients, nitrogen and phosphorous were also determined. Sample collected from animal waste storage had the highest estrogen concentration (98.7 ${\mu}g/L$), while sludge separated wastewater had the lowest concentration (3.4 ${\mu}g/L$). The mean concentrations of E2 and E1 in waste storage sample were (6.8 ${\mu}g/L$) and (68.7 ${\mu}g/L$), respectively. In sludge separated wastewater, the mean concentration of both E2 and E1 were reduced to (2.6 ${\mu}g/L$) and (1.9 ${\mu}g/L$), respectively. However, estriol was not detected in any of the samples collected. Mean ratios of E2 and E1 to macronutrients were significantly different between the methane wastewater and sludge separated wastewater owing to elimination of solid particles.

• Journal of Food Hygiene and Safety
• /
• v.21 no.4
• /
• pp.231-237
• /
• 2006

Nowadays the teabag is worldwide used for various products including green tea, tea, coffee, etc. since it is convenient for use. In case of outer packaging printed, however, there is a possibility that the plasticizers which is used for improvement in adhesiveness of printing ink may shift to inner tea bag. In this study, in order to monitor residual levels of plasticizers in teabags, we have established the simultaneous analysis method of 9 phthalates and 7 adipates plasticizers using gas chromatography (GC). These compounds were also confirmed using gas chromatography-mass spectrometry (GC-MSD). The recoveries of plasticizers analyzed by GC ranged from 82.7% to 104.6% with coefficient of variation of $0.6\sim2.7%$ and the correlation coefficients of each plasticizer was $0.9991\sim0.9999$. Therefore this simultaneous analysis method was showed excellent reproducibility and linearity. And limit of detection (LOD) and limit of quantitation (LOQ) on individual plasticizer were $0.1\sim3.5\;ppm\;and\;0.3\sim11.5\;ppm$ respectively. When 143 commercial products of teabag were monitored, no plasticizers analysed were detected in filter of teabag products. The migration into $95^{\circ}C$ water as food was also examined and the 16 plasticizers are not detected. In addition we carried out analysis of heavy metals, lead (Pb), cadmium (Cd), arsenic (As) and aluminum (Al) in teabag filters using ICP/AES. $Trace\sim23{\mu}g$ Pb per teabag and $0.6\sim1718{\mu}g$ Al per teabag were detected in materials of samples and Cd and As are detected less than LOQ (0.05 ppm). The migration levels of Pb and Al from teabag filter to $95^{\circ}C$ water were upto $11.5{\mu}g\;and\;20.8{\mu}g$ per teabag, respectively and Cd and As were not detected in exudate water of all samples. Collectively, these results suggest that there is no safety concern from using teabag filter.

• Korean Journal of Food Science and Technology
• /
• v.47 no.1
• /
• pp.27-36
• /
• 2015

The improved analytical method with gas chromatography (GC) and GC-mass spectrometry was established to identify and quantify disaccharides and trisacchrides in honey. In this method, the analysis of trimethylsilyl (TMS), TMS-oxime and TMS-methoxime sugars takes into account the determination of a single peak of complete separation on the chromatogram. The number of possible peaks for the qualitative and quantitative determination of TMS, TMS-oxime, and TMS-methoxime sugars was 17, 22, and 25, respectively. This new analytical method allowed for the determination of diand trisaccharides in honey by TMS-oxime and TMS-methoxime derivatives. This study suggested that the improved method is more suitable and precise than the other analytical methods for the simultaneous determination of sugars in honey.

• Journal of the Korea Academia-Industrial cooperation Society
• /
• v.16 no.12
• /
• pp.8836-8843
• /
• 2015

This study was performed to investigate the antiproliferative activities of supercritical extracts from phalsak(Citrus hassaku Hort ex Tanaka) and yeagam(Citrus iyo Hort. ex Tanaka) against human cervical carcinoma HeLa cells and the chemical compositions of the extracts. The anticancer properties of supercritical extracts were demonstrated using the MTT assay and Hoechst 33342 staining and the compositional analyses were conducted by using gas chromatography-mass spectrometry(GC-MS). The peel extracts of both species exhibited similar antiproliferative effect. The antiproliferative activity of the flesh extracts was not detected up to $400{\mu}g/mL$, whereas peel extracts of phalsak and yeagam reduced cell viability with 87.16% and 92.95% at $400{\mu}g/mL$, respectively. There was a dramatic increase of the apoptotic body formation in the cell treated with peel extracts while no apoptotic body formation detected in the cell treated with flesh extracts at 100, $200{\mu}g/mL$. By GC-MS analysis, 27 and 31 kinds of compounds identified in flesh and peel of phalsak, while 27 and 29 kinds of compounds were identified in flesh and peel of yeagam, respectively. 1,1,4,4-Tetramethyl-2-tetralone(20.86%), alloimperatorin(8.15%), limonene(11.23%), and auraptene(7.29%) were major in peel of phalsak, whereas limonene(22.19%), linalool(11.23%), and ${\gamma}$-sitosterol(9.12%) were major in peel of yeagam.

• Applied Biological Chemistry
• /
• v.51 no.3
• /
• pp.238-244
• /
• 2008

The essential oil was obtained from the aerial part of Caryopteris incana Miq. by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the essential oil were analyzed by gas chromatography-mass spectrometry (GCMS). The fragrance of the essential oil was fougere and woody. There were sixty-nine constituents in the essential oil: 28 carbohydrates, 22 alcohols, 7 acetates, 7 ketones, 3 aldehydes, and 2 others. Major constituents were 4,6,6-trimethyl [1S-($1{\alpha},2{\beta},5{\alpha}$)]-bicyclo[3.1.1]hept-3-en-2-ol (11.8%), taucadinol (9.4%), myrtenyl acetate (9.2%), pinocarvone (7.0%), 1-hydroxy-1,7-dimethyl-4-isopropyl-2,7-cyclodecadiene (6.3%), ${\delta}$-3-carene (6.2%). By SPME extraction, forty-nine constituents were identified: 22 hydrocarbons, 16 alcohols, 6 acetates, 3 ketones, and 2 ethers. Major constituents of the SPME-extracted sample were ${\delta}$-3-carene (12.6%), (-)-myrtenyl acetate (11.2%), 6,6-dimethyl-2-methylene-bicycol [3.1.1] heptan-3-o1 (10.9%), pinocarvone (9.3%). By HS extraction, ten constituents were identified: 5 hydrocarbons, 2 amines, 1 alcohol, and 2 others. Major constituents of the HS-extracted sample were (Z)-2-fluoro-2-butene (34.9%), ${\delta}$-3-carene (6.9%), 6-(4-chlorophenul)tetrahydro-2-methyl-2H-1,2-oxazine (5.9%). The $IC_{50}$ value (0.011 ${\mu}g/mg$) in MTT assay using HaCaT keratinocyte cell line was lower than those of commercially-selling rosemary and tea tree, suggesting more toxicological studies are needed for commercial use of the essential oil of Caryopteris incana Miq.