• Title/Summary/Keyword: fluorescence derivatization

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Detection of Foodborne Pathogens and Mycotoxins in Eggs and Chicken Feeds from Farms to Retail Markets

  • Lee, Minhwa;Seo, Dong Joo;Jeon, Su Been;Ok, Hyun Ee;Jung, Hyelee;Choi, Changsun;Chun, Hyang Sook
    • Food Science of Animal Resources
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    • v.36 no.4
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    • pp.463-468
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    • 2016
  • Contamination by foodborne pathogens and mycotoxins was examined in 475 eggs and 20 feed samples collected from three egg layer farms, three egg-processing units, and five retail markets in Korea. Microbial contamination with Salmonella species, Escherichia coli, and Arcobacter species was examined by bacterial culture and multiplex polymerase chain reaction (PCR). The contamination levels of aflatoxins, ochratoxins, and zearalenone in eggs and chicken feeds were simultaneously analyzed with high-performance liquid chromatography coupled with fluorescence detection after the post-derivatization. While E. coli was isolated from 9.1% of eggs, Salmonella species were not isolated. Arcobacter species were detected in 0.8% of eggs collected from egg layers by PCR only. While aflatoxins, ochratoxins, and zearalenone were found in 100%, 100%, and 85% of chicken feeds, their contamination levels were below the maximum acceptable levels (1.86, 2.24, and 147.53 μg/kg, respectively). However, no eggs were contaminated with aflatoxins, ochratoxins, or zearalenone. Therefore, the risk of contamination by mycotoxins and microbes in eggs and chicken feeds is considered negligible and unlikely to pose a threat to human health.

Development of a Simultaneous Detection and Quantification Method of Anorectics in Human Urine Using GC-MS and its Application to Legal Cases (GC-MS를 이용한 사람 뇨시료 중 비만치료제 분석 및 비만치료제 남용 현황의 법과학적 고찰)

  • Choi, Hyeyoung;Lee, Jaesin;Jang, Moonhee;Yang, Wonkyung;Kim, Eunmi;Choi, Hwakyung
    • YAKHAK HOEJI
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    • v.57 no.6
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    • pp.420-425
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    • 2013
  • Phentermine (PT) and phenmetrazine (PM) have been widely used as anti-obesity drugs. These drugs should be used with caution due to its close relation to amphetamine in its structure and toxicity. PT and PM, amphetamine-type anorectics, have recently been considered as alternatives for methamphetamine abuse in Korea. In addition, the misuse and abuse of PT and PM obtained by illegal sources such as the internet become a serious social problem. In the present study, a simultaneous detection and quantification method for determining PT and PM in human urine was developed and validated according to the international guidelines. The urine samples were screened using a fluorescence polarization immunooassay and analyzed by gas chromatography mass spectrometry (GC-MS) after extraction using automatic solid phase extraction (SPE) with a mixed-mode cation exchange cartridge and derivatization with pentafluoropropionic anhydride (PFPA). The validation results for selectivity, linearity, limits of detection (LOD) and quantification (LOQ), intra- and inter-assay precision and accuracy and recovery were satisfactory. The validated method was successfully applied to authentic urine samples collected from 38 drug abuse suspects. PT and/or PM were identified with or without methamphetamine in urine samples. Abuse of PT and PM have increased continuously in Korea, therefore, closer supervision of the inappropriate use of anoretics is necessary.

Analysis of Vitamin K1 in Commonly Consumed Foods in Korea (국내에서 소비되는 상용 식품의 비타민 K1 함량 분석)

  • Lee, Seongeung;Sung, Jeehye;Choi, Youngmin;Kim, Youngwha;Jeong, Heon-Sang;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.8
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    • pp.1194-1199
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    • 2015
  • Vitamin $K_1$ (phylloquinone) content of commonly consumed foods in Korea were determined by solvent extraction followed by reversed-phase liquid chromatography using post-column derivatization and fluorescence detection. Samples were obtained in the years of 2013 and 2015. In this study, 46 vegetables, 14 fruits, and 6 legumes were analyzed. Relatively higher amounts of vitamin $K_1$ were found in sweet potato leaves, green kiwi, and mung beans among vegetables, fruits, and legumes, respectively. The content of vitamin $K_1$ in vegetables including spinach, broccoli, and potato ranged from non-detectable (ND) to $1,467.3{\mu}g/100g$. The content of vitamin $K_1$ in fruits ranged from ND to $42.7{\mu}g/100g$. The content of vitamin $K_1$ in legumes, including soybeans, mung beans and peas ranged from 1.7 to $63.4{\mu}g/100g$. In addition, the analytical method validation parameters including recovery, reproducibility, repeatability, peak purity, and linearity were calculated to ensure the method's validity. The results showed high linearity with a correlation coefficient of 0.9999. Overall recovery was close to 100% (n=5). This study revealed reliable vitamin K content in commonly consumed foods in Korea for a nutritional information and food composition database.

Comparison of Extraction Methods for Determination of Vitamin K1 in Vegetables (채소류의 비타민 K1 분석을 위한 추출방법의 비교)

  • Kim, Hyeongi;Choi, Youngmin;Cho, Young-Sook;Sung, Jeehye;Ham, Hyeonmi;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.11
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    • pp.1791-1795
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    • 2014
  • The objective of this study was to compare two extraction methods for determination of vitamin K1 (phylloquinone) in vegetables. In addition, analytical method validation parameters such as accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and linearity were calculated to ensure the method's validity. Vitamin K1 was quantified by reversed-phase HPLC using post-column derivatization and fluorescence detection ($Ex{\lambda}=243nm$, $Ex{\lambda}=430nm$). Higher analytical values were observed using solvent extraction compared to those from the enzyme extraction method. The results from the method validation showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9994. The LOD and LOQ were 0.1335 and 0.2784 ng/injection volume ($50{\mu}L$), respectively. The inter-day precision and inter-day precision were 2.0% and 2.1%, respectively. Overall recovery was close to 100% (n=5). The phylloquinone contents ranged from 9.42 to $1,212.57{\mu}g/100g$. Our study provides reliable data on the phylloquinone contents in commonly consumed vegetables in Korea.

Distributions and Behaviors of H2O2 Above the Yellow Sea in the Years Between 2002 and 2004 (2002년에서 2004년 동안 서해상공에서 관측된 과산화수소의 농도분포 및 거동)

  • Kim Y.M.;Shin S.A.;Han J.S.;Lee M.H.;Kim J.A.
    • Journal of Korean Society for Atmospheric Environment
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    • v.21 no.6
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    • pp.689-697
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    • 2005
  • Hydrogen peroxide is a reservoir of OH radical which is the powerful oxidant in the atmosphere. Therefore, the status of the oxidizing atmosphere could be reflected on the concentration of $H_{2}O_{2}$. In this study, the distribution of $H_{2}O_{2}$ was determined during the intensive aircraft measurements over the Yellow sea in March, December 2002, April, November 2003 and March, October 2004. Flights covered from $124^{circ}E\;to\;129^{circ}E\;and\;35^{circ}N\;to\;37^{circ}N$, and extending to 3,000 m. The flight patterns were set properly to assess the altitudinal and longitudinal distribution for $H_{2}O_{2}$. $H_{2}O_{2}$ was extracted onto aqueous solution using a continuously flowing glass coil and analyzed by a high performance liquid chromatography (HPLC) accompanied with a fluorescence detector using postcolumn enzyme derivatization. Mixing ratios of $O_{3},\;NO_{x}\;and\;SO_{2}$ were measured in real time by commercial analysis instruments. Along the heights, the maximum concentration of $H_{2}O_{2}$ appeared around 1,500 m then gradually decreased with increasing altitude. The vertical behavior of ozone showed the similar trend to $H_{2}O_{2}$. The mean mixing ratio of $NO_{x}$ was about 2 ppbv and not showed clear vertical distribution patterns. The mean value of was the same as $NO_{x}$ however $SO_{2}$ appeared extreme concentration in low altitude. $H_{2}O_{2}\;and\;O_{3}$ showed even longitudinal distribution however $NO_{x}$ mixing ratio in land ($127^{circ}E$) was much higher than over the sea. $SO_{2}$ rather decreased with increasing longitude. $H_{2}O_{2}$ was in inverse proportion to $NO_{x}$ in spring and summer and $SO_{2}$ in spring, which indicated its significant role to NO and $SO_{2}$ oxidation pathways.

Studies on the Analysis of Benzo(a)pyrene and Its Metabolites on Biological Samples by Using High Performance Liquid Chromatography/Fluorescence Detection and Gas Chromatography/Mass Spectrometry

  • Lee, Won;Shin, Hye-Seung;Hong, Jee-Eun;Pyo, Hee-Soo;Kim, Yun-Je
    • Bulletin of the Korean Chemical Society
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    • v.24 no.5
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    • pp.559-565
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    • 2003
  • An analytical method the determination of benzo(a)pyrene (BaP) and its hydroxylated metabolites, 1-hydroxybenzo(a)pyrene (1-OHBaP), 3-hydroxybenzo(a)pyrene (3-OHBaP), benzo(a)pyrene-4,5-dihydrodiol (4,5-diolBaP) and benzo(a)pyrene-7,8-dihydrodiol (7,8-diolBaP), in rat urine and plasma has been developed by HPLC/FLD and GC/MS. The derivatization with alkyl iodide was employed to improve the resolution and the detection of two mono hydroxylated metabolites, 1-OHBaP and 3-OHBaP, in LC and GC. BaP and its four metabolites in spiked urine were successfully separated by gradient elution on reverse phase ODS $C_{18}$ column (4.6 mm I.D., 100 mm length, particle size 5 ㎛) using a binary mixture of MeOH/H₂O (85/15, v/v) as mobile phase after ethylation at 90 ℃ for 10 min. The extraction recoveries of BaP and its metabolites in spiked samples with liquid-liquid extraction, which was better than solid phase extraction, were in the range of 90.3- 101.6% in n-hexane for urine and 95.7-106.3% in acetone for plasma, respectively. The calibration curves has shown good linearity with the correlation coefficients (R²) varying from 0.992 to 1.000 for urine and from 0.996 to 1.000 for plasma, respectively. The detection limits of all analytes were obtained in the range of 0.01-0.1 ng/mL for urine and 0.1-0.4 ng/mL for plasma, respectively. The metabolites of BaP were excreted as mono hydroxy and dihydrodiol forms after intraperitoneal injection of 20 mg/kg of BaP to rats. The total amounts of BaP and four metabolites excreted in dosed rat urine were 3.79 ng over the 0-96 hr period from adminstration and the excretional recovery was less than 0.065% of the injection amounts of BaP. The proposed method was successfully applied to the determination of BaP and its hydroxylated metabolites in rat urine and plasma for the pharmacokinetic studies.

A Study on Contents of Vitamin K1 in Local Agricultural Products (지역농산물의 비타민 K1 함량 조사)

  • Lee, A Reum;Kim, Joo Hee;Park, Jae-Ho;Kim, Youngho;Hong, Eui Yon;Kim, Haeng-Ran;Choi, Youngmin;Lee, Junsoo;Eom, Hyun-Ju
    • The Korean Journal of Food And Nutrition
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    • v.29 no.3
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    • pp.301-306
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    • 2016
  • Vitamin K (phylloquinone) is an essential cofactor in the synthesis of active blood-clotting factors II, VII, IX and X. Deficiency of vitamin K leads to inadequate activity of these factors, resulting in bleeding. In this study, we investigated vitamin $K_1$ content of agricultural products that are widely and specifically grown in Korea including 9 leaves and vegetables, 16 fruits, and 11 cereals and specialty crops. Vitamin $K_1$ analysis of the agro-samples was by a validated, modified, reversed phase-HPLC method with fluorescence detection after post-column derivatization. The vitamin $K_1$ content ranged from 1.83 to $682.73{\mu}g$/100 g in leaves and vegetables, 0.17 to $28.22{\mu}g$/100 g in fruits, and ND to $279{\mu}g$/100 g in cereals and specialty crops. Among the 36 samples, high content of vitamin $K_1$ were found in Gugija (Lycium chinense Miller) leaves (average $682.73{\mu}g$/100 g) and Hansan ramie leaves (average $423.12{\mu}g$/100 g); however, mushroom, amaranth and Chinese artichoke showed no detectable levels. The results of ourstudy provide reliable vitamin $K_1$ content of Korean grown agricultural products that expand nutritional information and food composition database.

A Monitoring of Aflatoxins in Commercial Herbs for Food and Medicine (식·약공용 농산물의 아플라톡신 오염 실태 조사)

  • Kim, Sung-dan;Kim, Ae-kyung;Lee, Hyun-kyung;Lee, Sae-ram;Lee, Hee-jin;Ryu, Hoe-jin;Lee, Jung-mi;Yu, In-sil;Jung, Kweon
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.267-274
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    • 2017
  • This paper deals with the natural occurrence of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in commercial herbs for food and medicine. To monitor aflatoxins in commercial herbs for food and medicine not included in the specifications of Food Code, a total of 62 samples of 6 different herbs (Bombycis Corpus, Glycyrrhizae Radix et Rhizoma, Menthae Herba, Nelumbinis Semen, Polygalae Radix, Zizyphi Semen) were collected from Yangnyeong market in Seoul, Korea. The samples were treated by the immunoaffinity column clean-up method and quantified by high performance liquid chromatography (HPLC) with on-line post column photochemical derivatization (PHRED) and fluorescence detection (FLD). The analytical method for aflatoxins was validated by accuracy, precision and detection limits. The method showed recovery values in the 86.9~114.0% range and the values of percent coefficient of variaton (CV%) in the 0.9~9.8% range. The limits of detection (LOD) and quantitation (LOQ) in herb were ranged from 0.020 to $0.363{\mu}g/kg$ and from 0.059 to $1.101{\mu}g/kg$, respectively. Of 62 samples analyzed, 6 semens (the original form of 2 Nelumbinis Semen and 2 Zizyphi Semen, the powder of 1 Nelumbinis Semen and 1 Zizyphi Semen) were aflatoxin positive. Aflatoxins $B_1$ or $B_2$ were detected in all positive samples, and the presence of aflatoxins $G_1$ and $G_2$ were not detected. The amount of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in the powder and original form of Nelumbinis Semen and Zizyphi Semen were observed around $ND{\sim}21.8{\mu}g/kg$, which is not regulated presently in Korea. The 56 samples presented levels below the limits of detection and quantitation.