• Korean Journal of Pharmacognosy
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• v.52 no.4
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• pp.219-227
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• 2021

By analysing the benzo(a)pyrene concentration using HPLC-FLD and LC-MS/MS, pollution levels of herbal medicines without permitted benzo(a)pyrene specification were investigated. Average benzo(a)pyrene concentrations were 38.30, 37.46 and 21.22 ㎍/kg for Amomi Tsao-ko Fructus, Mume Fructus and Coptidis Rhizoma, respectively, which are 4 to 7 times higher than maximum permitted benzo(a)pyrene concentration of Rehmanniae Radix Preparata and Rehmanniae Radix, i.e. 5.0 ㎍/kg. Proportion of detected samples exceeding 5.0 ㎍/kg benzo(a)pyrene concentration was 22% for Cimicifugae Rhizoma and Scrophulariae Radix, 44% for Forsythiae Fructus, 67% for Mume Fructus, 100% for Amomi Tsao-ko Fructus and Coptidis Rhizoma, and collectively 29% (36 out of 125 samples) in average. In terms of risk characterization results, human exposure of benzo(a)pyrene were 7.96, 3.49 and 1.61 ng/kg b.w./day and the margin of exposure(MOE) were 1.25 × 10⁴, 2.86 × 10⁴ and 6.20 × 10⁴ for Mume Fructus, Amomi Tsao-ko Fructus and Coptidis Rhizoma, respectively. MOE banding of those herbal medicines was categorized to 'low concern'. However, considering that human exposure of benzo(a)pyrene for food is legislated to 1.4~2.5 ng/kg b.w./day, it was urgent to set up the guideline of benzo(a)pyrene in herbal medicines.

• 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.

• Korean Journal of Food Science and Technology
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• v.43 no.5
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• pp.544-552
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• 2011

The purpose of this study was to develop an analytical method for determining 15 polycyclic aromatic hydrocarbons (PAHs) of EU priority using gas chromatography (GC)-tandem mass spectrometry (MS). The PAHs in ground coffee were analyzed after being extracted using methods such as saponification-liquid-liquid extraction, Soxhlet extraction, and solid-liquid extraction. The solid-liquid extraction method showed the greatest repeatability and most efficient reduction of the matrix effect. GC-tandem MS for the quantification of the 15 PAHs showed better resolution and lower limit of detections (LODs) than GC-MS-selected ion monitoring (SIM) and high performance liquid chromatography with fluorescence detector. LODs of this method for the ground coffee types were 0.002-0.1 ${\mu}g/kg$ and limit of quantifications (LOQs) were 0.006-0.2 ${\mu}g/kg$ The recoveries ranged from 52.6 to 93.3%. Forty-six commercial types of ground coffee were analyzed to determine their PAHs contamination levels. PAHs concentration ranged from ND to 5.988 ${\mu}g/kg$. This study was conducted with toxicity equivalence factors, the U.S. EPA recommendation to identify dietary risks for PAHs in different types of coffee. The estimated average daily dose of PAHs was $5.24{\times}10^{-8}$ mg/kg body weight/day.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.151-160
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• 2015

This study was conducted to monitor residual pesticides in perilla leaf & lettuce and to assess their risk to human health. The total number of perilla leaf & lettuce were 4,063 and 2,248 respectively and these products were collected at the Garak-dong Agricultural & Marine Products Market sold by auction from 2010 to 2012. Multi-residual analysis of 285 pesticides were performed by GC-ECD, GC-NPD, HPLC-DAD and HPLC-FLD. In perilla leaf, 61 pesticides were detected and detection rate was 20.0%. 28 pesticides were detected in case of lettuce and detection rate was 4.8%. In order to do risk assessment by perilla leaf & lettuce consumption, estimated daily intake of residual pesticides were determined and compared to acceptable daily intake, referring to hazard index (HI values). The range of % HI values of perilla leaf was from 0.000% to 0.049%. The range of % HI values of lettuce was from 0.000% to 0.095%. These results show that the risk caused by pesticide residues in perilla leaf & lettuce intake were very low and these vegetable intake was safe.

• The Korean Journal of Pesticide Science
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• v.13 no.4
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• pp.216-222
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• 2009

The present study aims to monitor pesticide residues in cut flowers collected from the farms and markets. Cut flowers used in this study included rose, lily and chrysanthemum collected from June to September, 2008. Samples were collected once from farms in Hwasung, Goyang (Gyeonggi-do), Inje (Gangwon-do) and thrice from wholesale market in Namdaemunm, Yangjae and Gangnam (Seoul). Total of 24 pesticides (12 fungicides, 11 pesticides and 1 acaricide) were detected from samples collected from farm and total of 64 pesticides (25 fungicides, 36 pesticides, 1 acaricide and 2 fungicides) were detected from samples collected from wholesale market. The highest detection frequency of pesticide from farm was for carbaryl (15%) and for boscalid, fluacrypyrin, fluquinconazole, methomyl, pyraclostrobin, trifloxystrohin (10%), with overall detection of $0.1-36.99\;mg\;kg^{-1}$. While the highest detection frequency of pesticides from wholesale market was for carbaryl, fluquinoconazole and kresoxim-methyl (18.52%), methomyl (16.6%), and methiocarb and thiacloprid (12.96%) with overall detection amount of $0.1-56.2\;mg\;kg^{-1}$. Higher amount of pesticides were detected in leaves than in flowers. Among the pesticides detected, detection frequency of unregistered pesticides for rose, chrysanthemum and lily was 55%, 60% and 63% collected from farms and 47%, 60% and 89% collected from markets, respectively. These pesticides require registration and further monitoring in floricultural crops.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.329-335
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• 2017

Analysis method was presented for the simultaneous determination of nine bisphenol A related compounds such as bisphenol A (BPA), phenol, p-tert-butylphenol, bisphenol A diglycidyl ether (BADGE), $BADGE{\cdot}2H_2O$, $BADGE{\cdot}2HCl$, bisphenol F diglycidyl ether (BFDGE), $BFDGE{\cdot}2H_2O$ and $BFDGE{\cdot}2HCl$ migrated from inner coatings of metal food cans by high performance liquid chromatography (HPLC) with fluorescence detection. The method was validated by examining the linearity of calibration curve, the limit of detection (LOD), the limit of quantification (LOQ), recovery and uncertainty. The migration tests of nine BPA related compounds were carried out with four food simulants; deionized water (DW), 4% acetic acid, 50% ethanol and n-heptane. There was not any compound detected in DW, 4% acetic acid and 50% ethanol at $60^{\circ}C$ for 30 min and n-heptane at $25^{\circ}C$ for 60 min. BPA and phenol were migrated into 4% acetic acid and 50% ethanol at $95^{\circ}C$ for 30 min. The concentrations were ranged from 0 to $10.77{\mu}g/L$ of BPA and from 0 to $2.35{\mu}g/L$ of phenol. Canned foodstuffs mostly have long-term shelf life. We investigated migration of nine BPA related compounds according to the variation in storage periods (0~90 days) and temperatures (4, 25 and $60^{\circ}C$). All compounds were not founded during 90 days at $4^{\circ}C$ and $25^{\circ}C$, respectively. However BPA and $BADGE{\cdot}2H_2O$ were founded in DW and 4% acetic acid at $60^{\circ}C$. The migration levels of BPA and $BADGE{\cdot}2H_2O$ were close to the value of LOQ, respectively and did not change significantly as storage period. It was founded from results that the migration of BPA related compounds from metal food cans was controlled to a safe level.

• Natural Product Sciences
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• v.20 no.3
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• pp.160-169
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• 2014

44 compounds and 9 minerals were isolated from and detected in the New Zealand deer velvet antler Cervus elaphus var. scoticus L$\ddot{o}$nnberg. The chemical structures of (1 - 26) were identified on the basis of the spectroscopic methods and comparisons with literature, respectively. The structures were identified as cholesterol (CS, 6), 7-keto-CS (7), $7{\beta}$-hydroxy-CS (8), and $7{\alpha}$-hydroxy-CS (9), and included 12 steroid $3{\beta}$-O-(palmitic/stearic/myristic acid esters; PM/SA/MS) [CS-$3{\beta}$-O-PM (1 - 1), CS-$3{\beta}$-O-SA (1 - 2), CS-$3{\beta}$-O-MR (1 - 3), 7-keto-CS-$3{\beta}$-O-PM (2 - 1), 7-keto-CS-$3{\beta}$-O-SA (2 - 2), 7-keto-CS-$3{\beta}$-O-MR (2 - 3), $7{\beta}$-hydroxy-CS-$3{\beta}$-O-SA (3 -1), $7{\beta}$-hydroxy-CS-$3{\beta}$-O-PM (3 - 2), $7{\beta}$-hydroxy-CS-$3{\beta}$-O-MR (3 - 3), $7{\alpha}$-hydroxy-CS-$3{\beta}$-O-SA (4 - 1), $7{\alpha}$-hydroxy-CS-$3{\beta}$-O-PM (4 - 2), and $7{\alpha}$-hydroxy-CS-$3{\beta}$-O-MR (4 - 3)], dinonyl phthalate (5), 8 nucleic acids analogues [uracil (10), deoxyguanosine (11), deoxyuridine (12), uridine (13), deoxyadenosine (14), adenosine (15), inosine (16), and guanosine (17)], and the 9 free amino acids [L-phenylalanine (18), L-isoleucine (19), L-leucine (20), L-tyrosine (21), L-valine (22), L-proline (23), L-threonine (24), L-alanine (25), and L-hydroxyproline (26)]. Also, there are 8 kinds of amino acids [asparagine, serine, glutamine, glycine, histidine, arginine, methionine, and lysine], 2 sialic acids [N-acetylneuraminic acid (27), ketodeoxynonulosonic acid (28)], and 9 minerals [Na > K > Ca > Mg > Fe > Zn > B > Al > Cu] were detected from the autoaminoacid analyzer and ICP spectrometer, HPAEC-PAD/HPLC-FLD, respectively. 9 kinds of oxycholesterol-$3{\beta}$-O-fatty acid ester (2 - 1, 2 - 2, 2 - 3, 3 - 1, 3 - 2, 3 - 3, 4 - 1, 4 - 2, and 4 - 3) and 3 nucleic acids (12, 14, and 15) were isolated from the velvet antler for the first time. 6 kinds of steroids (7, 8, 9, 2 - 1, 3 - 1, and 4 - 1) were examined for their anti-proliferative effects against L1210, P388D1, K562, MEG-01, KG-1, MOLT-4, A549, HepG2, MCF-7, SK-OV-3, and SW-620 cancer cell lines. They showed anti-proliferative effects with $IC_{50}$ values of 0.06, 2.16, 2.42, > 50.0, 1.66 and $8.31{\mu}M$ against L1210, while the values were 24.05, 9.44, 5.22, 0.25. 9.48 and $49.77{\mu}M$ against P388D1, respectively. The others were inactive.

• Journal of Food Hygiene and Safety
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• v.29 no.3
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• pp.170-180
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• 2014

The aim of this study was to investigate pesticide residues in 2,877 market vegetables in the northern area of Seoul in 2013. Pesticide residues in the samples were analysed by multiresidue method for 285 pesticides using GC-ECD/NPD and HPLC-DAD/FLD. 385 samples(13.4%) were detected with pesticide residues at or below MRL, and 15 samples(0.5%) were found to detect pesticide residues exceeding MRL. The most frequently detected samples were sedum(63.6%), chamnamul(45.8%), leek(44.5%) and green&red pepper(30.8%). Among the 15 violated samples, leek(5 cases) and welsh onion(4 cases) showed the highest violation rate. A total of 74 samples(18.5%) contained multiple pesticide residues in one vegetable. Procymidone, chlorofenapyr and cypermethrin were the pesticide most frequently found. 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 into the range of 1.05~28.61%. The results have meant that there was no health risk through dieting commercial agricultural products detected with pesticide residues.

• The Korean Journal of Pesticide Science
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• v.14 no.4
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• pp.381-393
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• 2010

In order to monitor the residual characteristics of the pesticides in leafy vegetables selling at wholesale markets and traditional markets in Cheongju, a total of 180 samples of 15 leafy vegetables, such as broccoli, celery, chard, chicory, Chinese vegetable, Chwinamul, crown daisy, Korean cabbage, leek, lettuce, perilla leaves, Shinsuncho, spinach, welsh onion and young radish, were purchased from the wholesale markets and traditional markets in June and August in 2010 and the pesticide residues in them were analyzed by multiresidue analysis method using GLC, HPLC and GC-MSD. Seven pesticides were detected from 12 samples out of total 180 samples collected, representing detection rate was 6.7%. In case of the samples collected from markets in June, four pesticides including tefluthrin were detected from six samples and in case of the samples collected from markets in August, three pesticides including pendimethalin were detected from three samples. The MRL-exceeding rate of pesticides detected from leafy vegetables was 0.6%. The pesticide exceeded its MRL was azoxystrobin detected from crown daisy and many pesticides were not registered to the crops, excepting that azoxystrobin detected from Chwinamul and tefluthrin from leek. Estimated daily intakes (EDIs) of the pesticides detected from leafy vegetables were less than 7% of their acceptable daily intakes (ADIs), representing that residue levels of the pesticides detected were evaluated as safe.