• Title/Summary/Keyword: method detection limit

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The Study on the Methylmercury Analysis and the Monitoring of Total Mercury and Methylmercury in Fish (어류 중 메틸수은 분석법 확립 및 모니터링)

  • Kim, Hee-Yun;Chung, So-Young;Sho, You-Sub;Oh, Geum-Soon;Park, Seong-Soo;Suh, Jung-Hyuk;Lee, Eun-Ju;Lee, Yoon-Dong;Choi, Woo-Jeong;Eom, Ji-Yoon;Song, Min-Soo;Lee, Jong-Ok;Woo, Gun-Jo
    • Korean Journal of Food Science and Technology
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    • v.37 no.6
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    • pp.882-888
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    • 2005
  • Procedure for analysis of methylmercury in fish was developed, involving addition of HCl, extraction with toluene, and clean-up using L-cystein solution. Obtained extract is analyzed by gas chromatography with electron capture detector using Ulbon HR-Thermon-Hg column. Detection limit and recovery of the method were 0.005mg/kg (expressed as Hg), 98-107 (103%), respectively. Total mercury and methylmercury concentrations in 175 commercial fish samples ranged from [mean-max (mean), unit: mg/kg]: 0.014-1.200 (0.270) and 0.006-0.901 (0.168) in tuna-fish, 0.020-0.934 (0.323) and 0.012-0.553 (0.149) in martin-fish, 0.082-0.782 (0.391) and 0.040-0.436(0.201) in shark, 0,023-0.031 (0.026) and 0,013-0.018 (0.015) in salmon, 0.098-0.193 (0.133) and 0.031-0.015(0.090) in tilefish, and 0,031-0.214 (0.089) and 0.016-0.093 (0.042) in canned tuna respectively. No sample of analyzed fish exceeded 1.0mg/kg wet wt., limit for methylmercury established by Codex. In all species examined, estimated weekly intake was lower than Provisional Tolerable Weekly Intake recommended by the JECFA (the Joint FAO/WHO Expert Committee on Food Additives).

Simultaneous Determination of Aminoglycoside Antibiotics in Meat using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS를 이용한 육류 중 아미노글리코사이드계 항생제 9종의 동시분석 및 적용성 검증)

  • Cho, Yoon-Jae;Choi, Sun-Ju;Kim, Myeong-Ae;Kim, MeeKyung;Yoon, Su-Jin;Chang, Moon-Ik;Lee, Sang-Mok;Kim, Hee-Jeong;Jeong, Jiyoon;Rhee, Gyu-Seek;Lee, Sang-Jae
    • Journal of Food Hygiene and Safety
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    • v.29 no.2
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    • pp.123-130
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    • 2014
  • A simultaneous determination was developed for 9 aminoglycoside antibiotics (amikacin, apramycin, dihydrostreptomycin, gentamicin, hygromycin B, kanamycin, neomycin, spectinomycin, and streptomycin) in meat by liquid chromatography tandem mass spectrometry (LC-MS/MS). Each parameter was established by multiple reaction monitoring in positive ion mode. The developed method was validated for specificity, linearity, accuracy, and precision based on CODEX validation guideline. Linearity was over 0.98 with calibration curves of the mixed standards. Recovery of 9 aminoglycosides ranged on 60.5~114% for beef, 60.1~112% for pork and 63.8~131% for chicken. The limit of detection (LOD) and limit of quantification (LOQ) were 0.001~0.009 mg/kg and 0.006~0.03 mg/kg, respectively in livestock products including beef, pork and chicken. This study also performed survey of residual aminoglycoside antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Aminoglycosides were not found in any of the samples.

Determination of $^{14}C$ in Environmental Samples Using $CO_2$ Absorption Method ($Co_2$ 흡수법에 의한 환경시료중 $^{14}C$ 정량)

  • Lee, Sang-Kuk;Kim, Chang-Kyu;Kim, Cheol-Su;Kim, Yong-Jae;Rho, Byung-Hwan,
    • Journal of Radiation Protection and Research
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    • v.22 no.1
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    • pp.35-46
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    • 1997
  • A simple and precise method of $^{14}C$ was developed to analyze $^{14}C$ in the environment samples using a commercially available $^{14}CO_2$ absorbent and a liquid scintillation counter. An air sampler and a combustion system were developed to collect HTO and $^{14}CO_2$ in the air and the biological samples simultaneously. The collection yield of $^{14}CO_2$ by the air sampler was in the range of 73-89% . The yield of the combustion system was 97%. In preparing samples for counting, the optimum ratio of $CO_2$ absorbent to the scintillator for mixing was 1:1. No variation of the specific activity of $^{14}C$ in the counting sample was observed up to 70 days after preparation of the samples. The detection limit for$^{14}C$ was 0.025 Bq/gC, which is the level applicable to the natural level of $^{14}C$. The analytical result of $^{14}C$ obtained by the present method were within ${\pm}6%$ of the relative error from the one by the benzene synthesis. The specific activity of $^{14}C$ in the air collected at Taejon during the period of October 1996 ranged from 0.26 to 0.27 Bq/gC. The specific activity of $^{14}C$ in the air collected at 1km from the Wolsong nuclear power plant a 679 MWe PHWR, was $0.54{\pm}0.03$ Bq/gC. The ranges of specific activities of $^{14}C$ in the pine needles and the vegetations from the areas around the Wolsong nuclear power plant were 0.56-0.67 Bq/gC and 0.23-1.41 Bq/gC, respectively.

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Selective determination of mercury (II) ion in aqueous solution by chemiluminescence method (화학발광법에 의한 수용액 중의 선택적 수은(II) 이온 정량)

  • Kim, Kyung-Min;Jang, Taek-Gyun;Kim, Young-Ho;Oh, Sang-Huyb;Lee, Sang-Hak
    • Analytical Science and Technology
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    • v.24 no.4
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    • pp.243-248
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    • 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 $1.25{\times}10^{-7}M$.

The Monitoring of Heavy Metals in Human Bloods of Middle School Students (중학생의 혈액 중 중금속 모니터링)

  • Park Hee Ra;Kim Meehye;Kwun Ki-Sung;Kim Soon Ki;Heo Su-Jeong;Kim Kwang_Jin;Yum Tae-Kyung;Choi Kwang Sik;Kim Soo Yeon
    • Journal of Food Hygiene and Safety
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    • v.20 no.2
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    • pp.83-88
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    • 2005
  • This study was conducted to estimate the contents of heavy metals including lead, cadmium, zinc, copper as well as iron status(serum iron, total iron binding capacity, feritin etc)in blood samples of middle school students(n=300). The contents of heavy metals were determined using the GF-AAS (Graphite furnace Atomic Absorption Spectrophotometer). The microwave digestion method and dilution method were compared. The dilution method showed the better recovery and detection limit than microwave digestion method. The values of toxic metals in whloe blood of boys & girls were 3.46 & 3.05 for Pb,0.063 & 0.065 for Cd respectively (ug/dL). Also the values of trace metals in serum of boys & girls were 105.9 & 92.6 for Zn, 98.3 & 99.0 for Cu respectively (ug/dL). The prevalence of iron deficiency was $7.5\%$ in 146 boys and $14.3\%$ in 156 girls. The mean values of lead in girls were higher in iron deficiency, iron deficiency anemia and anemia groups than normal group. The mean values of lead and zinc were higher in boys compared to those in girls(P<0.05), the mean values of cadmium and copper in boys were similar to those in girls. Our results of toxic metals such as Pb & Cd showed lower to CDC's(Centers for Disease Control) blood lead levels of concern for children, 10 ug/dL.

Monitoring of Uniconazole by GC-NPD (GC-NPD 동시분석법을 이용한 유니코나졸 잔류실태조사)

  • Kim, Eun-Jeung;Choi, Bu-Chuhl;Choi, Su-Jeong;Hong, Chae-Kyu;Kim, Eun-Hee;Choi, Chae-Man;Seo, Young-Ho;Hwang, Young-Sook;Jang, Mi-Ra;Hwang, In-Sook;Kim, Moo-Sang;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.378-381
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    • 2012
  • The monitoring of the uniconazole residual pesticide for agricultural products was conducted by multiclass pesticide multiresidue methods. Samples were collected from June to November, 2011. Uniconazole pesticide was detected in 49 samples from a total of 3,939 samples. The amount of uniconazole pesticide ranged from 0.09 to 17.89 mg/kg in 49 samples. This method was described for the simultaneous determination of uniconazole by gas chromatography with a nitrogen phosphorus detector (GC-NPD) and mass spectrometry (MS). The limit of detection and quantification were 0.006 and 0.018 mg/kg GC-NPD, respectively. For an evaluation of the GC-NPD method, uniconazole spiked into gyeojachae at a level of 0.5, 5 mg/kg was determined. The recoveries of uniconazole by the GC-NPD method ranged from 83.4 to 101.4%. The results indicate that the method of simultaneous analysis is applicable to uniconazole analysis.

Establishment of an Analytical Method for Novobiocin in Livestock Products Using HPLC-UVD (HPLC-UVD를 이용한 축산식품 중 Novobiocin의 시험법 확립)

  • Park, Hee-Ra;Kwon, Chan-Hyeok;Lee, Jong-Goo;Kim, Hyung-Soo;Chae, Young-Sik;Oh, Jae-Ho;Kwon, Ki-Sung
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.263-268
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    • 2012
  • Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.

Development of Analysis Method of Caffeine and Content Survey in Commercial Foods by HPLC (HPLC를 이용한 카페인의 분석법 개발 및 시판 식품중 함유량 조사)

  • Kim, Hee-Yun;Lee, Young-Ja;Hong, Ki-Hyoung;Lee, Chul-Won;Kim, Kil-Saeng;Ha, Sang-Chul
    • Korean Journal of Food Science and Technology
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    • v.31 no.6
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    • pp.1471-1476
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    • 1999
  • A simple and practical method for determination of caffeine in foods was developed. The analysis of caffeine was performed by reverse phase high performance liquid chromatography using a ${\mu}-Bondapak\;C_{18}$ column at isocratic condition with methanol-acetic acid-water(20 : 1 : 79) on UV detector at 280 nm. The clean-up and extraction of caffeine in samples were based on a simple pretreatment using a Sep-Pak $C_{18}$ cartridge. Recovery rates obtained with this method for cider, candy, cookie, milk, ice cream and persimmon leaf tea were 99.23%, 99.50%, 99.17%, 99.37%, 98.93% and 99.10% respectively. And the detection limit of caffeine was $0.1\;{\mu}g/mL$. With this method, the range of caffeine contents extracted from coffee, green tea, black tea, Oolong tea(tea bag), soft drinks, ice cream, milk and commercial confectionery were $3.38{\sim}37.50\;mg/g,\;16.30{\sim}26.10\;mg/g,\;10.80{\sim}16.65\;mg/g,\;11.25\;mg/g,\;0.06{\sim}0.11\;mg/g,\;0.04{\sim}0.44\;mg/g,\;0.04{\sim}0.39\;mg/g\;and\;0.10{\sim}1.80\;mg/g$, respectively. But caffeine was not detected in the other tea such as Acanthopanax sessiliflorum tea, Angelica gigas tea, Angelica tea, Arrow root tea, Duchu'ng tea, Dunggulle tea, Ganoerma lucidum tea, Ginger tea powder, Persimmon leaf tea, Ssanghwa tea and Cocoa mix powder.

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A Study on Searching for Export Candidate Countries of the Korean Food and Beverage Industry Using Node2vec Graph Embedding and Light GBM Link Prediction (Node2vec 그래프 임베딩과 Light GBM 링크 예측을 활용한 식음료 산업의 수출 후보국가 탐색 연구)

  • Lee, Jae-Seong;Jun, Seung-Pyo;Seo, Jinny
    • Journal of Intelligence and Information Systems
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    • v.27 no.4
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    • pp.73-95
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    • 2021
  • This study uses Node2vec graph embedding method and Light GBM link prediction to explore undeveloped export candidate countries in Korea's food and beverage industry. Node2vec is the method that improves the limit of the structural equivalence representation of the network, which is known to be relatively weak compared to the existing link prediction method based on the number of common neighbors of the network. Therefore, the method is known to show excellent performance in both community detection and structural equivalence of the network. The vector value obtained by embedding the network in this way operates under the condition of a constant length from an arbitrarily designated starting point node. Therefore, it has the advantage that it is easy to apply the sequence of nodes as an input value to the model for downstream tasks such as Logistic Regression, Support Vector Machine, and Random Forest. Based on these features of the Node2vec graph embedding method, this study applied the above method to the international trade information of the Korean food and beverage industry. Through this, we intend to contribute to creating the effect of extensive margin diversification in Korea in the global value chain relationship of the industry. The optimal predictive model derived from the results of this study recorded a precision of 0.95 and a recall of 0.79, and an F1 score of 0.86, showing excellent performance. This performance was shown to be superior to that of the binary classifier based on Logistic Regression set as the baseline model. In the baseline model, a precision of 0.95 and a recall of 0.73 were recorded, and an F1 score of 0.83 was recorded. In addition, the light GBM-based optimal prediction model derived from this study showed superior performance than the link prediction model of previous studies, which is set as a benchmarking model in this study. The predictive model of the previous study recorded only a recall rate of 0.75, but the proposed model of this study showed better performance which recall rate is 0.79. The difference in the performance of the prediction results between benchmarking model and this study model is due to the model learning strategy. In this study, groups were classified by the trade value scale, and prediction models were trained differently for these groups. Specific methods are (1) a method of randomly masking and learning a model for all trades without setting specific conditions for trade value, (2) arbitrarily masking a part of the trades with an average trade value or higher and using the model method, and (3) a method of arbitrarily masking some of the trades with the top 25% or higher trade value and learning the model. As a result of the experiment, it was confirmed that the performance of the model trained by randomly masking some of the trades with the above-average trade value in this method was the best and appeared stably. It was found that most of the results of potential export candidates for Korea derived through the above model appeared appropriate through additional investigation. Combining the above, this study could suggest the practical utility of the link prediction method applying Node2vec and Light GBM. In addition, useful implications could be derived for weight update strategies that can perform better link prediction while training the model. On the other hand, this study also has policy utility because it is applied to trade transactions that have not been performed much in the research related to link prediction based on graph embedding. The results of this study support a rapid response to changes in the global value chain such as the recent US-China trade conflict or Japan's export regulations, and I think that it has sufficient usefulness as a tool for policy decision-making.

Evaluation for Application of IOM Sampler for Agricultural Farmer's Inhalation Exposure to Kresoxim-methyl and Fenthion (농작업자의 Kresoxim-methyl과 fenthion에 대한 호흡노출량 측정을 위한 IOM 채집기의 효율성 평가)

  • Lee, Jiho;Kim, Eunhye;Lee, Jonghwa;Shin, Yongho;Maasfeld, Wolfgang;Choi, Hoon;Moon, Joon-Kwan;Lee, Hyeri;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.230-240
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    • 2015
  • An IOM sampler equipped with glass fiber filter has been recently utilized instead of solid adsorbent, which was used to measure the inhalation exposure of agricultural operator to pesticides. The aim of this study is to validate the efficacy of an IOM sampler by measuring the trapping efficiency and breakthrough using kresoxim-methyl water-dispersible granule and fenthion emulsifiable concentrate. On LC-MS/ MS, minimum detection level was 12.5 pg and method limit of detection was 5.0 ng/mL. Good linearity ($R^2$ > 0.999) for matrix matched standards was obtained. Recoveries of pesticides from glass fiber filter were 102-109% (kresoxim-methyl) and 97-104% (fenthion) while those from XAD-2 resin were 94-98% (kresoxim methyl) and 93-100% (fenthion). Trapping efficiency test was performed with personal air pumps and IOM sampler (glass fiber filter) connected with solid adsorbent (XAD-2 resin) with two types of formulation (solid and liquid) which were diluted by standard rate and sprayed to IOM sampler. Those pesticides were trapped only in glass fiber filter without any breakthrough to solid adsorbent. After spiking of pesticides to glass fiber filter, breakthrough test was carried out with IOM sampler (glass fiber filter) which was connected with solid adsorbent. As a results, 87-101% of kresoxim-methyl and 96-105% of fenthion remained in spiked glass fiber filter, however, no pesticides were detected in second glass fiber filter and solid adsorbent. In conclusion, IOM sampler which equipped with glass fiber filter can be applied widely for pesticide inhalation exposure study since it has good trapping efficiency and adsorption capacity, regardless of the solid or liquid formulation.