The aim of this study was to determine total mercury and methyl mercury level in fishes (Deep-sea Fish, Tuna, Billfish) and fishery products. A total of 101 fishes and 44 fishery products samples collected from commercial market in Gyeonggi-do. Total mercury were analysed by mercury analyzer and methyl mercury were analyzed by gas chromatography with electron capture detector. In the fishes, total mercury was detected in all samples and methylmercury was detected in 92 samples of them. The detection rate of methylmercury was 91.1% in fishes. The mean concentration (mg/kg) of total mercury and methylmercury were $1.968{\pm}0.505/0.496{\pm}0.057$ for Billfish, $0.665{\pm}0.091/0.252{\pm}0.033$ for Deep-sea Fish and $0.577{\pm}0.085/0.218{\pm}0.025$ for Tuna, respectively. The Swordfish contains the highest level of total mercury (1.968 mg/kg) and methylmercury (0.496 mg/kg). In Mabled rockfish, the ratio of methylmercury's contents about total mercury's contents was the highest as 66.5%. In case of fishery products, frozens made of 100% of raw material contained the highest level of total mercury and methyl mercury. The weekly intake of total mercury and methylmercury was calculated in 4.72% and 5.24% of Provisional Tolerable Weekly Intake (PTWI) respectively. This study showed that the weekly intake of methylmercury from Deep-sea Fish, Tuna and Billfish was less than the PTWI recommended by the Joint FAO/WHO expert committee on food additives.
Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.
Kim, Kyung-Min;Jang, Taek-Gyun;Kim, Young-Ho;Oh, Sang-Huyb;Lee, Sang-Hak
Analytical Science and Technology
/
v.24
no.4
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pp.243-248
/
2011
A selective determination method of mercury (II) ion in aqueous solution by luminol-based chemiluminescence system (luminol CL system) has been developed. Determination of metal ions such as copper (II), iron (III), chromium (III) ion in solution by the luminol CL system using its catalytic role in the reaction of luminol and hydrogen peroxide has been reported by several groups. In this study, the catalytic activity of mercury (II) ion in the reaction of luminol and hydrogen peroxide was observed by the enhanced CL intensity of the luminol CL system. Based on this phenomenon, experimental conditions of the luminol CL system were investigated and optimized to determine mercury (II) ion in aqueous solution. While mercury (II) ion in mixed sample solution containing mercury (I) and (II) ions highly enhanced the CL intensity of the luminol CL system, the mercury (I) ion could not enhanced the CL intensity. Thus selective determination of the mercury (II) ions in a mixture containing mercury (I) and (II) ions could be achieved. Each concentration of mercury (I) and (II) ions in aqueous solution can be obtained from the results of the CL method that give the concentration of only mercury (II) ion and the inductively coupled plasma (ICP) method that give the total concentration of mercury ions. On the optimized conditions, the calibration curve of mercury (II) ion was linear over the range from $1.25{\times}10^{-5}$ to $2.50{\times}10^{-3}M$ with correlation coefficient of 0.991. The detection limit of mercury (II) ion in aqueous solution was calculated to be $1.25{\times}10^{-7}M$.
Journal of the Korean Society of Food Science and Nutrition
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v.42
no.10
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pp.1618-1628
/
2013
Relationships between fatty acids and tocopherols in conventional and genetically modified peanut cultivars were studied by gas chromatography with flame ion detector and high performance liquid chromatography with fluorescence detection. Eight fatty acids and four tocopherol isomers in the sample set were identified and quantified. Oleic acid and linoleic acid are major fatty acids and the ratio of oleic and linoleic acids ranged from 1.11 to 16.26. Tocopherols contents were 6.76 to 12.24 for ${\alpha}$-tocopherol (T), 0.08 to 0.39 for ${\beta}$-T, 5.28 to 15.02 for ${\gamma}$-T, and 0.17 to 1.17 mg/100 g for ${\delta}$-T. Correlation coefficient (r) for fatty acids and tocopherols indicated a strong inverse relationship between oleic & linoleic acids (r=-0.97, P<0.05) and positive relationships between palmitic & linoleic acids (r=0.95, P<0.05) and ${\gamma}$-T & ${\delta}$-T (r=0.83, P<0.05). Principal component analysis (PCA) of fatty acids and tocopherols gave four significant principal components (PCs, with eigenvalues>1), which together account for 85.49% of the total variance in the data set with PC1 and PC2 contributing 45.27% and 21.33% of the total variability, respectively. Eigen analysis of the correlation matrix loadings of the four significant PCs revealed that PC1 was mainly contributed by palmitic, oleic, linoleic, and gondoic acids, while PC2 was by behenic acid, ${\beta}$-T, and ${\gamma}$-T. The score plot generated by PC1-PC2 identified sample clusters in the two spatial planes based on the oleic and linoleic acids. The score plot PC3-PC4 didn't separate sample groups.
This study's purpose is to present the improvement of effectiveness of security activity for international conference among Several Countries which can be held hereafter. On the basis of security activity problems originating in APEC that had been held in Busan in 2005. I made up questions three times to on the members of the police, military, fire figher and national intelligence service who had experienced in Busan APEC and recognition of possible problem and possibility of improvement on each item of questions was analyzed by Delphi Method. Also interviews with 4 security experts selected from each security agency were conducted to present improvement in each part of problem. The results obtained from the face to face interview with four experts of security-enforcement agency about the role and importance of site activity stage for international conference among several countries are as followings ; First, the system that experienced security-enforcement agents can be selected for the next national security event is needed, by data-basing the security-enforcement agents who were experienced in security event as man power management. Second, the middle-term plan for the introduction of high-tech equipment and joint inspection with relevant security agents are needed for the efficient explosive technical detection. Third, high-tech security equipment could be introduced through the international high-tech security equipment exhibition. Fourth, an anti-terrorism plan should be measured by sharing information through the cooperation with domestic and international intelligence agency. Fifth, public relations should be measured systematically by organization rather than agents' individual public relations. Sixth, political consideration to secure integrative coordination with other agency is needed for security activity, through normal cooperation with fire fighting related agency such as an electric, gas, elevator company. Seventh, a definite press guideline is needed for a convenient news coverage and safety during security event.
Backgrounds: The measurement of volume of isoflow has been considered as a sensitive test for detecting small airway diseases showing normal pulmonary function in a routine pulmonary function test. To evaluate the functions of small airway among dust exposed workers, the changes of volume of isoflow were measured and its applicability of managing early stage pneumoconiosis patients was studied. Method: The subjects were 67 male, pneumoconiosis with small opacity and FEV1>80%, FEV1/FVC>75% in spirometry and the controls were 20 male, no dust-exposed office workers. The maximal epiratory volume curves after inhalation of indoor air and $He-O_2$ gas mixtures were measured and ${\Delta}V_{max50},\;{\Delta}V_{max75},\;V_{iso}V/VC$ between the dust exposed and control workers were compaired. Results: 1) There were no significant differences between two group in ${\Delta}V_{max50}$ and ${\Delta}V_{max75}$. But the ratio of $V_{iso}V/VC$ of the subjects was siginificantly higher than that of the control (p<0.01). This study confirms that $V_{iso}V/VC$ is a very useful index in early detection of small airway dysfunction. 2) The ratio of $V_{iso}V/VC$ of the subjects was signigicantly different between only smoker group and mixed group(smoker and nonsmoker). It suggestes that smoking is an important cousative factor of small airway dysfunction. 3) As the profusion of the chest X-ray increased, the rartio of $V_{iso}V/VC$ increased, but no significant difference of $V_{iso}V/VC$ was found between categories of pneumoconiosis. The categories of pneumoconiosis and small airway dysfunction may not be related. 4) No significant relationship was established between the duration of work and the ratio of $V_{iso}V/VC$. Conclusions : It is concluded that the measurement of $V_{iso}V/VC$ is useful to detect small airway dysfuction of early stage pnuemoconiosis patents with small opacities but showing normal pulmonary function in a routine pulmonary function test.
The aim of this study was to determine the methylmercury (MeHg) levels in abyssal fish species. The MeHg in the fishes was extracted with hydrochloric acid and toluene and then purified using an L-cysteine solution. The extract was analyzed with a gas chromatography-electron capture detector (GC-${\mu}ECD$) with a thermon Hg-capillary column. The detection limit and the recovery of the method were 0.002 and 84.2-98.5% (mean, 93.4%), respectively. The MeHg content in 492 abyssal fishes ranged from 0.037 to 2.009 mg/kg. The levels of MeHg [range, mg/kg (mean)] were significantly dependent on fish species and presented as the following; 0.157-2.009 (0.546) in Scalloped hammerhead shark, 0.211-0.878 (0.501) in Blue shark, 0.121-0.993 (0.482) in Spiny dogfish, 0.243-0.658 (0.397) in Salmon shark, 0.074-1.958 (0.353) in Blacktip shark, 0.038-0.807 (0.302) in Southern hake, 0.099-0.511 (0.300) in Scorpion fish, and 0.037-0.133 (0.067) in Ling. The monitoring results showed that the estimated weekly intake of MeHg from sharks, Southern hake, and Ling were lower than the provisional tolerable weekly intake recommended by the Joint FAO/WHO expert committee on food additives.
The method for the determination of ethylenediamine (EDA) and hexamethylenediamine (HMDA) in food simulants was developed, and migration amounts of these compounds was monitored for 124 polyamide (PA) utensils. The diurethane derivatives of EDA and HMDA, which produced by reaction with ethyl chloroformate, were analyzed by using gas chromatograph (GC)/flame ionization detector (FID) and GC/mass spectrometer (MS). The developed method was validated with $0.3\;{\mu}g/mL$ of limit of detection (LOD) for EDA and $0.1\;{\mu}g/mL$ of LOD for HMDA, > 0.999 of linearity($r^2$) and > 88% of recovery. The EDA was detected 1.31 and $02.06\;{\mu}g/mL$ for 2 samples in water. The HMDA was detected $0.29\;-\;0.93\;{\mu}g/mL$ for 3 samples in 20% ethanol and $0.26\;-\;0.44\;{\mu}g/mL$ for 10 samples in n-heptane. These migration levels were below the specific migration limits (SML) of $12\;{\mu}g/mL$ and $2.4\;{\mu}g/mL$ for EDA and HMDA established in EU.
Yun, Sang Soon;Lee, Sang Jin;Lim, Do Yeon;Lim, Ho Soo;Lee, Gunyoung;Kim, MeeKyung
Journal of Food Hygiene and Safety
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v.32
no.5
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pp.381-388
/
2017
In this study, we investigated the levels of natural preservatives of benzoic acid, sorbic acid, and propionic acid in spices. The quantitative analysis was performed using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for benzoic acid and sorbic acid and gas chromatography-mass spectrometry (GC-MS) for propionic acid. The sample was extracted with ethanol using sonication, then centrifuged and evaporated to dryness and redissolved to 1 mL with ethanol to use for the instrumental analysis. The analytical method was validated based on linearity, recovery, limit of detection (LOD), and limit of quantification (LOQ). This method was suitable to determine low amounts of naturally occurring preservatives (benzoic acid, sorbic acid, and propionic acid) in various spices. Benzoic acid, sorbic acid, and propionic acid were found in 165 samples, 88 samples, and 398 samples, respectively from the total of 493 samples. The concentration of benzoic acid, sorbic acid, and propionic acid were ranged at ND-391.99 mg/L, ND-57.70 mg/L, and ND-188.21 mg/L in spices, respectively. The highest mean levels of benzoic acid, sorbic acid, and propionic acid were found in cinnamon (167.15 mg/L), basil leaves (22.79 mg/L), and white pepper (51.48 mg/L), respectively. The results in this study provide ranges of concentration regarding naturally occurring benzoic acid, sorbic acid, and propionic acid in spices. Moreover, the results may use to the case of consumer complaint or trade friction due to the inspection services of standard criteria for the preservatives of spices.
This study was conducted to analyze the microbial community and propionic acid production ability of natural microflora in the rice cakes. Genetic analysis of natural microflora in Jorangyi rice cake was performed to select propionic acid - producing bacteria. Selected propionic acid-producing bacteria were cultivated in TSB (tryptic soy broth) supplemented with glucose, and growth characteristics were analyzed by temperature and production of propionic acid was analyzed by gas chromatography (GC-FID). Linearity, detection limit, quantitative limit, and recovery rate were measured to verify propionic acid assay. A total of 98 microbial strains were detected from microflora of Joraengyi rice cake that grew after expiration of shelf life. Lactobacillus casei group accounted for 50.48% and Lactobacillus buchneri was 29.60%. Propionic acid - producing bacteria were Propionibacterium thoenii, P. cyclohexanicum, Propionibacterium_uc, P. jensenii, and P. freudenreichii. Natural bacteria and Lactobacillus spp. did not produce propionic acid during 14 days but P. cyclohexanicum, P. freudenreichii subsp. Shermanii, P. thoenii and P. jesenii produced $263.47{\mu}g/mL$, $338.90{\mu}g/mL$, $325.43{\mu}g/mL$ and $222.17{\mu}g/mL$ during 4 days and 2,462.02 and 2,904.78, 2,220.64, $3,519.17{\mu}g/mL$ during 14 days. As a result of this study, it was affirmed that the natural microflora of Joraengyi rice cake during storage can produce propionic acid from natural sources even if a high concentration of propionic acid is not intentionally added. Because of characteristics of rice cake composed of starch and glucose. This study will be used as a recognition criterion to detect natural preservatives such as propionic acid in starchy foods such as rice cakes and as reference standard safety management data.
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