• 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.

• Journal of Food Hygiene and Safety
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• v.28 no.1
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• pp.75-82
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• 2013

The simultaneous analysis and monitoring of aflatoxin $B_1$, $G_1$, $B_2$, $G_2$ and ochratoxin A in foods were carried out by HPLC with fluorescence detection. The samples were extracted with methanol/water mixture. The extract was centrifuged, diluted with phosphate buffer saline (PBS), filtered, and applied to an immunoaffinity column containing antibodies specific to both aflatoxins and ochratoxin A. After washing the column with PBS and water, the toxins were eluted from the column with methanol, and quantified by HPLC, with a run time of approximately 30 min. The recoveries for aflatoxin $B_1$, $G_1$, $B_2$, $G_2$ and ochratoxin A in foods were 78.4~101.5%, 73.3~102.1%, 81.7~106.7%, 67.0~104.6% and 78.7~120.8%, respectively. The limits of detection of aflatoxins and ochratoxin A ranged from 0.05 to $0.18{\mu}g/kg$. According to monitoring result with the established method, aflatoxin $B_1$ and ochratoxin A were found in 13 of 151 domestic commercial foods. The contamination levels were $0.32{\sim}1.80{\mu}g/kg$ for aflatoxin $B_1$ and $0.97{\mu}g/kg$ for ochratoxin A. Therefore, this study showed all commercial foods monitored were safe under the Korean standards for aflatoxins and ochratoxin A.

• Journal of Food Hygiene and Safety
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• v.26 no.4
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• pp.315-321
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• 2011

This study was performed to investigate contamination levels of aflatoxins, the secondary metabolites produced by fungi Aspergillus flavus and A. parasiticus, in herbal medicine. Herbs is susceptible to these fungi infections through its growth harvest, transport and storage. This study determine the aflatoxin $B_1$, $B_2$, $G_1$ and $G_2$ levels by HPLC-florescence detector coupled with photochemical enhancement in 558 samples herbal medicine distributed in Korea and China. Also, We checked a transfer ratio of aflatoxins from raw herbal medicines to herbal medicine extract. Hot water extraction of herbal medicines was prepared by air pressure and high pressure condition. The analytical method for aflatoxins was validated in this method. In results recoveries of the analytical method were ranged from 67.4% to 96.2% and, limits of detection and quantitation for aflatoxins were $0.015{\sim}0.138\;{\mu}g/kg$ and $0.046{\sim}0.418\;{\mu}g/kg$, respectively. According to the results of monitoring on aflatoxins in herbal medicine, aflatoxins 1.7 ug/kg $B_1$ and 0.9 ug/kg $G_1$ were detected in only one sample of Strychni Ignatii Semen, and 0.8 ug/kg $G_1$ in Strychni Semen. About 13.6~51.3% of aflatoxins were transferred to hot water extract. Although the detected levels are under the permitted levels for aflatoxins in herbal medicine, these amounts should be considered in regard to overall daily exposure to mycotoxins.

• Journal of Food Hygiene and Safety
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• v.21 no.2
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• pp.76-81
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• 2006

We optimized conditions of extract solvents and elution solvents for total aflatoxins in foods using HPLC/FLD. The extract solvent was 70% methanol solution including 1% NaCl and the 3 mL of acetonitrile was used as elution solvent using immnuoaffinity column. The detection limits (LOD) was 0.05 ng/g. The recoveries for total aflatoxins ($B_1,\;B_2,\;G_1\;and\;G_2$) studied in foods were cereals ($74.1{\sim}95.5%,\;83.7{\sim}98.8%,\;80.4{\sim}102.4%,\;72.8{\sim}76.5%$), pulses ($85.8{\sim}87.5%,\;83.8{\sim}90.7%,\;92.0{\sim}94.5%,\;60.6{\sim}65.6%$), nuts ($84.6{\sim}97.1%,\;86.0{\sim}94.1%,\;95.5{\sim}111.5%,\;71.0{\sim}89.9%$), processed foods ($81.5{\sim}87.1%,\;82.8{\sim}85.8%,\;85.4{\sim}92.7%,\;68.9{\sim}76.4%$), dried fruits ($83.6{\sim}93.5%,\;78.1{\sim}90.4%,\;93.0{\sim}108.5%,\;64.9{\sim}78.5%$) and other foods ($72.5{\sim}98.3%,\;73.1{\sim}96.4%,\;83.5{\sim}107.2%,\;64.2{\sim}75.8%$), respectively.

• Korean Journal of Environmental Agriculture
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• v.32 no.1
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• pp.61-69
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• 2013

BACKGROUND: This survey was done to investigate the pesticide residues and to assess their risk on agricultural products on the Markets in Incheon from 2010 to 2012. METHODS AND RESULTS: The total number of samples were 16,025 for agricultural products and these were analyzed by multi-residue method using GC-ECD/NPD, GC-MS, LC-MS/MS and HPLC-PDA/FLD. The violation rates of the samples over maximum residue limits(MRLs) of pesticide residues established by Korean Food and Drug Administration in the survey of 2010, 2011 and 2012 were 1.2%, 0.8% and 0.7%, respectively. CONCLUSION(S): Of the total violated samples, more than 75% of the rates were recorded from the samples of leafy vegetables. Most commonly encountered agricultural commodities over MRLs were Chwinamul, perilla leaves and crown daisy. The pesticides detected yearly over MRLs during three years were endosulfan, chlorpyrifos, diazinon, lufenuron, chlorothalonil, flutolanil, procymidone, ethoprophos. Estimated daily intakes compared to acceptable daily intakes, except radish and Welsh onion, is estimated less harm on human in 10 kinds of pesticides which frequently occurred violation.

• The Korean Journal of Pesticide Science
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• v.12 no.1
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• pp.24-33
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• 2008

In this study, the mobility of seven pesticides from soil in different slopes was investigated by simulated rainfall under field conditions. Simulated rainfall subjected to $22\;mm\;hr^{-1}$ was treated using rainfall simulator after 12 hr of pesticide treatment. Amounts of the pesticides were measured in run-off water samples. The soil samples collected before and after rainfall from upper, middle and lower parts and three different depths of sloped-plot were also analyzed. At result, the order of the amount of pesticide residues was $0{\sim}15$ > $15{\sim}30$ > $30{\sim}45\;cm$ of soil depth and no pattern was shown in upper, middle and lower, and different slopes in soil samples. all pesticides from the run-off water samples collected from soils were detected maximum 96% within 60 minutes after first collection except carbendazim and cypermethrin which have the lowest water solubilities. These results revealed that mobility of pesticides can be dependant mainly on soil textures and physicochemical properties of pesticides. Therefore, it can be suggested that selection of pesticides should be considered for properties of pesticide in the alpine and sloped-land.

• Korean Journal of Environmental Agriculture
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• v.33 no.2
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• pp.111-120
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• 2014

BACKGROUND: This study was conducted to investigate the levels of pesticide residues in fruits and to assess their risk to human health. METHODS AND RESULTS: Monitoring of 215 samples of fruits collected from local markets in incheon during 2013 was performed. 259 pesticides were analyzed by multi-residue method and Quick, Easy, Cheap, Effective, Rugged, and safe/Mass/Mass(QuEChERS/MS/MS) method using Gas Chromatography-Electron Capture Detector/Nitrogen Phosphorus Detector(GC-ECD/NPD), GC-MS, LC(Liquid Chromatography-Mass/Mass(LC-MS/MS) and High Performance Liquid Chromatography-Photodiode Array/Fluorescence Detector(HPLC-PDA/FLD). In 56.3% of the samples detected pesticide residues and were not found to exceed Maximum Residue Limits(MRL). The highest detected samples were found in citrus fruits(83.9%). Among the detected compounds, carbendazim(13.1%), imazalil (11.7%), thiabendazole(10.7%) and fludioxonil(9.8%) were frequently found in fruits. A risk assessment of pesticide residues in fruits was performed by calculating Estimated Daily Intake(EDI) and Acceptable Daily Intake(ADI). Also, we were evaluated removal efficiency of pesticide residues by washing and peeling. The removal efficiency of pesticide residues in citrus and tropical fruits by peeling processes were 91.6%. After the washing process, the removal rates were 43.1%(Cherry, Grape, Blueberry). CONCLUSION: The level of pesticide residues in fruits was within the MRL. The range of %ADI values was from 0.00011 to 0.98795%. The process of washing or peeling reduces the level of pesticide residues. The results of this research concluded that the detected pesticides are not harmful to human being.

• Journal of Food Hygiene and Safety
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• v.23 no.4
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• pp.319-323
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• 2008

Analytical method for determination of florfenicol was developed for estimate veterinary drug residue of unestablished MRLs in meat. The method was validated in correspondence with the CODEX guideline for florfenicol residue in meat. The samples mixed with sodium sulfate were extracted with ethyl acetate. After clean-up, the residue was dissolved in mobile phase and analyzed using high-performance liquid chromatography with fluorescence detector. The calibration curve showed good linearity($r^2=0.9997$) within the concentration range of $0.05{\sim}1.0\;mg/kg$. The limit of detection(LOD) and limit of quantification(LOQ) were validated at 0.012 and 0.039 mg/kg, respectively. The recoveries in fortified meat ranged from 85.6 to 95.6%($1.1{\sim}5.3%$ RSD) at the 0.05 to 0.4 spiking levels. We monitored 150 samples of meats that were purchased in Korea(Seoul, Busan, Daegu, Daejeon and Gwangju). Among tested samples, florfenicol was detected in 1 of pig at the level of 0.040 mg/kg, and below LOQ in 1 of cattle, 2 of pig and 2 of chicken. The residues of florfenicol in the tested samples were within the MRLs.

• Korean Journal of Food Science and Technology
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• v.44 no.2
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• pp.235-239
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• 2012

This research was conducted to monitor ochratoxin A in wine, beer, $makgeolli$ and fermented alcoholic beverages to estimate the exposure to ochratoxin A in the assorted alcoholic beverages. The analytical method for ochratoxin A was based on immuno-affinity column clean up followed by HPLC-FLD. Ochratoxin A was detected in 30 samples of 177 wine (17%), 25 samples of 106 beer (23.6%), 11 samples of 74 $makgeolli$ (14.9%), and 7 samples of 74 fermented alcoholic beverages (9.5%). The average levels of ochratoxin A were 0.039 ng/mL in wine, 0.010 ng/mL in beer, 0.023 ng/mL in $makgeolli$, and 0.014 ng/mL in fermented alcoholic beverages. The daily dietary exposure level of ochratoxin A estimated by using the report on national health and nutrition survey were 0.039 ng/b.w.day from wine, 0.010 ng/b.w.day from beer, 0.023 ng/b.w.day from $makgeolli$, and 0.014 ng/b.w.day from fermented alcoholic beverage.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.7
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• pp.1035-1040
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• 2015

4-Hexylresorcinol (4-HR) has been used for prevention of melanosis in shrimp. Recently, 4-HR in EU and other countries was authorized with maximum residue levels of 1~2 mg/kg but remains unauthorized in Korea. Therefore, the aim of this study was to investigate the effect of 4-HR on melanosis inhibition and residual levels in Korean shrimp according to various concentrations and soaking times. We previously reported that the HPLC-FLD method can be used for detection of 4-HR at maximum levels of 1~2 mg/kg in shrimp. Our results show that residual levels of 4-HR in peeled and unpeeled shrimps were in the range of 0.86 to 13.46 mg/kg and 0.02 to 2.33 mg/kg, respectively. In addition, 4-HR treatment at concentrations of 10 and 20 mg/L for 72 h were effective for inhibition of melanosis in peeled shrimp compared with unpeeled shrimp. These results provide basic data for the establishment of guidelines and regulation related to 4-HR.