• Title/Summary/Keyword: Safety Curve

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Development and Validation of Analytical Method for Wogonin, Quercetin, and Quercetin-3-O-glucuronide in Extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus Mixture (연잎, 상엽, 건조 무 혼합 추출물의 지표성분 wogonin, quercetin 및 quercetin-3-O-glucuronide의 분석법 개발 및 검증)

  • Jang, Gill-Woong;Park, Eun-Young;Choi, Seung-Hyun;Choi, Sun-il;Cho, Bong-Yeon;Sim, Wan-Sup;Han, Xinggao;Cho, Hyun-Duk;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.289-295
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    • 2018
  • The aim of this study was to develop and validate an analytical method for determining the presence of wogonin, quercetin, and quercetin-3-O-glucuronide in extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus mixtures. We evaluated the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of analytical methods for wogonin, quercetin, and quercetin-3-O-glucuronide using high performance liquid chromatography. Our result showed that the correlation coefficients of the calibration curve for wogonin, quercetin, and quercetin-3-O-glucuronide were 0.9999. The LOD for wogonin, quercetin, and quercetin-3-O-glucuronide ranged from 0.09 to 0.16 and those for the LOQ ranged from 0.26 to $0.48{\mu}g/mL$. The inter-day and intra-day precision values of wogonin, quercetin, and quercetin-3-O-glucuronide ranged from 0.74 to 1.87 and from 0.28 to 1.12%, respectively. The inter-day and intra-day accuracies were 99.96~115.88% and 99.73~114.81%, respectively. Therefore, the analytical method was validated for the detection of wogonin, quercetin, and quercetin-3-O-glucuronide in extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus mixtures.

Effect of Hot Water and Microwave Heating on the Inactivation of Enterobacter sakazakii in Reconstituted Powdered Infant formula and Sunsik (열수(熱水)와 마이크로웨이브 가열이 조제분유 및 선식 용해 중 Enterobacter sakazakii 사멸에 미치는 영향)

  • Kim, Jung-Beom;Park, Yong-Bae;Lee, Myung-Jin;Kim, Ki-Cheol;Huh, Jeong-Weon;Kim, Dae-Hwan;Lee, Jong-Bok;Kim, Jong-Chan;Choi, Jae-Ho;Oh, Deog-Hwan
    • Journal of Food Hygiene and Safety
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    • v.23 no.2
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    • pp.157-162
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    • 2008
  • Enterobacter sakazakii was initially referred to as yellow-pigmented Enterobacter cloacae and reclassified in 1980. E. sakazakii infection cause life-threatening meningitis, septicemia, and necrotizing enterocolitis in infants. Powdered infant formula (PIF) and baby foods may be the important vehicle of E. sakazakii infection. It has been reported that E. sakazakii was isolated from PIF and sunsik ingredients produced in Korea. Some infants have been fed sunsik as a weaning diet. Therefore, it is necessary that this organism should be inactivated on preparing PIF and sunsik at homes and in hospitals. The cocktail of three Korean E. sakazakii strains (human, sunsik and soil isolates) were used to investigate the inactivation of this organism with hot water at 50, 60, 65, 70 and $80^{\circ}C$ and microwave heating for 60, 75, 90, 105 and 120 sec. Reconstituted PIF and sunsikwere inoculated with cocktailed vegetative cells of E. sakazakii at 6 log CFU/mL. Thermal inactivation of vegetative cells of E. sakazakii were achieved by reconstituted PIF and sunsik with hot water at $60^{\circ}C$ or greater and with microwave heating at 2,450 MHz for 75 sec or longer. Considering that biofilm formation of E. sakazakii was adapted to survive the dry environment that is PIF and sunsik and thermal resistance increased, it is suggested that inactivation of E. sakazakii was used by hot water at $70^{\circ}C$ or greater and microwave heating for 90 sec or longer. Reconstituted PIF and sunsik were inoculated with cocktailed vegetative cells of E. sakazakii at 2 to 3 log CFU/mL to investigate the growth curve of this organism and stored at 5, 10, 15, 20, 25, 30 and $35^{\circ}C$. Viable counts slightly changed at 5, $10^{\circ}C$ during 48 h but grew at $15^{\circ}C$ or greater. Considering that E. sakazakii is able to grow in infant formula milk at refrigerator temperature, reconstituted PIF and sunsik that are not immediately consumed should be discarded or stored at refrigeration temperatures within 24 h.

Studies on Simultaneous Determination of Chlorophyll a and b, Pheophorbide a, and $\beta-Carotene$ in Chlorella and Spirulina Products (클로렐라 및 스피루리나제품에 함유된 엽록소 a, b, 페오포르바이드 a 및 $\beta$-카로틴의 동시분석법에 관한 연구)

  • Lee Young Ja;Kim So Hee;Kim Jin-Sook;Han Jeong A;Seo Hae Jeom;Lim Hyo Jeong;Choi Soo Young
    • Journal of Food Hygiene and Safety
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    • v.20 no.3
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    • pp.141-146
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    • 2005
  • A simple and sensitive analysis method based on reverse phase (RP) HPLC with UV detector was developed for simultaneous determination of chlorophyll a and b, pheophorbide a and $\beta-Carotene$ in Chlorella and Spirulina products. For added concentration $(50\;\mug/ml)$ of chlorophyll a and b, pheophorbide a and $\beta-Carotene$, recoveries of those were 70.3, 71.6, 60.1 and $90.5\%$, respectively, with relative standard deviations of 2.8,6.0, 10.6 and $10.4\%$. Limit of detection and quantification had ranges of $0.1\sim1.0\;\mug/ml$ and $0.2\sim2.0\;\mug/ml$, respectively. Calibration curve was linear with correlation coefficient of 0.995 for chlorophyll a and b, pheophorbide a and $\beta-Carotene$. Results of simultaneous determination in Chlorella and Spirulina products were showed ranges of $121.g\sim543.0\;\mug/ml$ for chlorophyll a,$0.6\sim160.0\;\mug/ml$ for chlorophyll b, $19.2\sim60.3\;\mug/ml$ for pheophorbide a and $383.6\sim1713.7\;\mug/ml$ for $\beta-Carotene$, respectively. Chlorophyll b contents in Chlorella products were detected above 30 times level to those in Spirulina products. $\beta-Carotene$ contents in Spirulina products were detected 2.7 times level to those in Chlorella products.

Development of Analytical Methods of Spinosad in Agricultural Commodities by HPLC with UV Detector and Monitoring (HPLC-UVD를 이용한 농산물 중 스피노사드 분석법 개선 및 잔류실태 조사)

  • Kim, Hee-Yun;Choi, Sun-Hee;Chung, So-Young;Choi, Hee-Ju;Kim, Yong-Hoon;Cho, Min-Ja;Seo, Eun-Chae;Han, Kyoung-Jin;Choi, Jae-Chun;Park, Hee-Ok;Ha, Sang-Chul;Shin, Il-Shik;Eom, Ji-Yoon
    • Korean Journal of Food Science and Technology
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    • v.43 no.2
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    • pp.125-133
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    • 2011
  • The purpose of this study was to develop a methodology to detect spinosad which are difficult to analyze by multi-component simultaneous analysis of pesticide residues. We monitored spinosad due to the paucity of related information. The spinosad was determined using HPLC with UV detector at 250 nm. Correlation coefficient ($r^2$) for standard curve of spinosad A and D at standard concentration of 0.1-5.0 mg/kg were 0.999, respectively. Limit of quantitation (LOQ) of HPLC analysis was 0.005 mg/kg while limit of detection (LOD) was 0.001 mg/kg. Recovery experiments were conducted on five representative agricultural products to validate the analytical method. The recovery of proposed methods ranged from 74.9% to 104.0% and relative standard deviations were less than 10%. Spinosad residues were investigated in 16 commodities collected from 22 provinces. In this study, residues on all samples were not detected.

Monitoring and Risk Assessment of Pesticide Residues on Stalk and Stem Vegetables Marketed in Incheon Metropolitan Area (인천광역시 유통 엽경채류 농산물의 잔류농약 실태조사 및 위해성 평가)

  • Park, Byung-Kyu;Jung, Seung-Hye;Kwon, Sung-Hee;Ye, Eun-Young;Lee, Han-Jung;Seo, Soon-Jae;Joo, Kwang-Sig;Heo, Myung-Je
    • Journal of Food Hygiene and Safety
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    • v.35 no.4
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    • pp.365-374
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    • 2020
  • This study was conducted to monitor the residual pesticides on a total of 320 stalk and stem vegetables from January 2019 to December 2019 in the Incheon metropolitan area. Pesticide residues in samples were analyzed by the multi-residue method for 373 pesticides using GC-MS/MS, LC-MS/MS, GC-ECD, GC-NPD and HPLC-UVD. Risk assessment was also carried out based on the amount of stalk and stem vegetables consumed. The linearity correlation coefficient for the calibration curve was 0.9951 to 1.0000, LOD 0.002 to 0.022 mg/kg, LOQ 0.005 to 0.066 mg/kg and recovery was 82.0 to 108.0%. According to the monitoring of pesticides, 36 (11.3%) of 320 were detected with pesticide residues and 3 (0.9%) samples exceeded the maximum residual limit. The detection frequency for Chinese chives and Welsh onion was higher than that for other stalk and stem vegetables. The frequently detected pesticides were etofenprox, procymidone, fludioxonil, and pendimethalin. As a tool of risk assessment through the consumption of pesticide detectable agricultural products, the ratio of estimated daily intake (EDI) to acceptable daily intake (ADI) was calculated in the range of 0.0062-24.1423%. These results indicate that there is no particular health risk through consumption of commercial stalk and stem vegetables detected with pesticide residues.

A Study on the Analysis of Five Artificial Sweetners in Beverages by HPLC/MS/MS (HPLC/MS/MS를 이용한 음료류 중 인공감미료 동시분석에 관한 연구)

  • Lee, Seong-Bong;Yong, Kum-Chan;Hwang, Sun-Il;Kim, Young-Su;Jung, You-Jung;Seo, Mi-Young;Lee, Chang-Hee;Sung, Jin-Hee;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.29 no.4
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    • pp.327-333
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    • 2014
  • A method for analysis of five artificial sweetners (sodium saccharin, aspartame, acesulfame-K, sucralose, cyclamate) in beverage samples was developed using high-performance liquid chromatography/triple quadrupole mass spectrometry (HPLC/MS/MS). The method uses a single-step dilution for sample preperation. Seperation was achieved on a $C_{18}$ column ($2.1{\times}150mm$, $3.5{\mu}m$) with A- 2% methanol (1 mM ammonium acetate), B-95% methanol (1 mM ammonium acetate) as mobile phase with gradient mode. The quantitation of target compounds was performed by external calibration in selected reaction monitorning (SRM) mode. The coefficient of determination of calibration curve for sodium saccharin, aspartame, acesulfame-K, sucralose and cyclamate were 0.9957, 0.9991, 0.9943, 0.9982 and 0.9948, respectively. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 0.001~0.022 mg/L and 0.004~0.073 mg/L, repectively. Recoveries for beverage samples were in the range of 92.76~113.50% with RSD < 10.91%. The method has applied to the determination of the five sweetners in 102 beverage samples. Three artificial sweetners-aspartame, acesulfame-K, sucralose were detected from 42 samples. Sodium saccharin and cyclamate were not detected in all samples.

Improvement of Fatigue Life with Local Reinforcement for Offshore Topside Module during Marine Transportation (해양플랫폼 탑사이드 모듈의 해상 운송 시 국부 보강을 통한 피로 수명 개선에 관한 연구)

  • Jang, Ho-Yun;Seo, Kwang-Cheol;Park, Joo-Shin
    • Journal of the Korean Society of Marine Environment & Safety
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    • v.27 no.2
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    • pp.387-393
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    • 2021
  • In this study, finite element analysis was performed to evaluate a method of increasing the fatigue life of the pipe connection structure commonly used in the topside structure of offshore platforms. MSC Patran/Nastran, a commercial analysis program, was used, and the critical structural model was selected from the global analysis. To realize the stress concentration phenomenon according to the load, modeling using 8-node solid elements was implemented. The main loads were considered to be two lateral loads and a tensile load on a diagonal pipe. To check the hotspot stress at the main location, a 0.01 mm dummy shell element was applied. After calculating the main stress at the 0.5-t and 1.5-t locations, the stress generated in the weld was estimated through extrapolation. In some sections, this stress was observed to be below the fatigue life that should be satisfied, and reinforcement was required. For reinforcement, a bracket was added to reduce the stress concentration factor where the fatigue life was insufficient without changing the thickness or diameter of the previously designed pipe. Regarding the tensile load, the stress in the bracket toe increased by 23 %, whereas the stress inside and outside of the pipe, which was a problem, decreased by approximately 8 %. Regarding the flexural load, the stress at the bracket toe increased by 3 %, whereas the stress inside and outside of the pipe, which was also a problem, decreased by approximately 48 %. Owing to the new bracket reinforcement, the stress in the bracket toe increased, but the S-N curve itself was better than that of the pipe joint, so it was not a significant problem. The improvement method of fatigue life is expected to be useful; it can efficiently increase the fatigue life while minimizing changes to the initial design.

Monitoring and Risk Assessment of Pesticide Residues in School Foodservice Agricultural Products in Gwangju Metropolitan Area (광주광역시 학교급식 농산물의 잔류농약 모니터링 및 위해평가)

  • Kim, Jinhee;Lee, Davin;Lee, Mingyou;Ryu, Keunyoung;Kim, Taesun;Gang, Gyungri;Seo, Kyewon;Kim, Jung-Beom
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.283-289
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    • 2019
  • This study was performed to monitor the residual pesticides in agricultural products used in school foodservice in the Gwangju metropolitan area. Risk assessment was also carried out based on the amount of agricultural products consumed. A total of 320 agricultural products supplied to schools in Gwangju were analyzed from 2015 to 2017. The pre-treatment and residual pesticide analysis of these products was conducted in accordance with the second method for multi-residue analysis of pesticides in the Korean food code. The hazard index was calculated by dividing the estimated daily intake (EDI) of pesticides by the acceptable daily intake (ADI). The linearity correlation coefficient for the calibration curve was 0.9923 to 1.0000, LOD 0.004 to 0.019 mg/kg, LOQ 0.012 to 0.057 mg/kg, and recovery was 79.1 to 100.2%. Residual pesticides were detected in 18 (5.6%) of 320 agricultural products used for school foodservice, and one sample of sweet potato stem (0.3%) exceeded the maximum residual limit (MRL). The detection frequency for chili peppers and bell peppers was higher than that for other agricultural products. The frequently-detected pesticides were boscalid and acetamiprid. These results showed that residual pesticide management is needed for chili pepper, bell pepper and sweet potato stem among agricultural products supplied to schools. The hazard index of bifenthrin in sweet potato stem showed the highest (64.18%), and the other pesticides were 0.03-8.23%. These results indicated that agricultural products supplied to schools in Gwangju were safe for consumption. To minimize the intake of residual pesticides, it is necessary to not only thoroughly wash agricultural products but to also ensure the expanded supply of products that are pesticide-free.

Development and Validation of Analytical Method and Antioxidant Effect for Berberine and Palmatine in P.amurense (황백의 지표성분 berberine과 palmatine의 분석법 개발과 검증 및 항산화 효능 평가)

  • Jang, Gill-Woong;Choi, Sun-Il;Han, Xionggao;Men, Xiao;Kwon, Hee-Yeon;Choi, Ye-Eun;Park, Byung-Woo;Kim, Jeong-Jin;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.35 no.6
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    • pp.544-551
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    • 2020
  • The aim of this study was to develop and validate a simultaneous analytical method for berberine and palmatine, which are representative substances of Phellodendron amurense, and to evaluate the antioxidant activity. We evaluated the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of analytical methods for berberine and palmatine using high-performance liquid chromatography. Our result showed that the correlation coefficients of the calibration curve for berberine and palmatine exhibited 0.9999. The LODs for berberine and palmatine were 0.32 to 0.35 µg/mL and the LOQs were 0.97 to 1.06 µg/mL, respectively. The inter-day and intra-day precision values for berberine and palmatine were from 0.12 to 1.93 and 0.19 to 2.89%, respectively. The inter-day and intra-day accuracies were 98.43-101.45% and 92.39-100.60%, respectively. In addition, the simultaneous analytical method was validated for the detection of berberine and palmatine. Moreover, we conducted FRAP and NaNO2 scavenging activity assays to measure the antioxidant activities of berberine and palmatine, and both showed antioxidant activity. These results suggest that P.amurense could be a potential natural resource for antioxidant activity and that the efficacy can be confirmed by investigating the content of the berberine and palmatine.

Modification and Validation of an Analytical Method for Dieckol in Ecklonia Stolonifera Extract (곰피추출물의 지표성분 Dieckol의 분석법 개선 및 검증)

  • Han, Xionggao;Choi, Sun-Il;Men, Xiao;Lee, Se-jeong;Oh, Geon;Jin, Heegu;Oh, Hyun-Ji;Kim, Eunjin;Kim, Jongwook;Lee, Boo-Yong;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.37 no.3
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    • pp.143-148
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    • 2022
  • This study was to investigate an analytical method for determining dieckol content in Ecklonia stolonifera extract. According to the guidelines of International Conference on Harmonization. Method validation was performed by measuring the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of dieckol using high-performance liquid chromatography-photodiode array. The results showed that the correlation coefficient of calibration curve (R2) for dieckol was 0.9997. The LOD and LOQ for dieckol were 0.18 and 0.56 ㎍/mL, respectively. The intra- and inter-day precision values of dieckol were approximately 1.58-4.39% and 1.37-4.64%, respectively. Moreover, intra- and inter-day accuracies of dieckol were approximately 96.91-102.33% and 98.41-105.71%, respectively. Thus, we successfully validated the analytical method for estimating dieckol content in E. stolonifera extract.