• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.13-21
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• 2019

A method was developed for the simultaneous detection of an antibiotic fungicide, streptomycin, and its metabolite (dihydrostreptomycin) in agricultural products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using methanol adjusted to pH 3 using formic acid, and purified with a HLB (Hydrophilic lipophilic balance) cartridge. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.001 to 0.1 mg/kg, and linearity of five agricultural products (hulled rice, potato, soybean, mandarin, green pepper), with coefficients of determination $(R^2){\geq}0.9906$, for streptomycin and dihydrostreptomycin. The mean recoveries at three fortification levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) were from 72.0~116.5% and from 72.1~116.0%, and relative standard deviations were less than 12.3% and 12.5%, respectively. The limits of quantification (LOQ) were 0.01 mg/kg, which are satisfactory for quantification levels corresponding with the Positive List System. All optimized results satisfied the criteria ranges requested in the Codex guidelines and the Food Safety Evaluation Department guidelines. The present study could serve as a reference for the establishment of maximum residue limits and be used as basic data for detection of streptomycin and dihydrostreptomycin in food.

• Journal of Applied Biological Chemistry
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• v.57 no.3
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• pp.235-242
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• 2014

The purpose of this study is the establishment of scientific processes for making food safety policies. Thus, we investigated pesticide residue level of the agricultural commodities from market, and performed risk assessment. Fifteen agricultural items are chosen based on the frequency of Korean consumption. The samples were collected from 9 cities where populations are more than one million. Total 283 active ingredients were monitoring ( total sample number =232). Single-analysis of target pesticides was for three kinds of possible growth regulators and the multicomponent analysis was for 280 kinds of pesticides, a total of 283 species were selected to perform the pesticide residues. Before monitoring the analytes, the improvements of the analytical methods were done by method validations under the CODEX analytical method development guidelines and can produce metrics that represent the international standards applied in accordance with the guidelines. In addition to residual pesticides detected during monitoring we compare the ADI to EDI values using detected result and dietary consumption data which is extracted from annual market basket survey. The 163 samples were non-detected in the total 232 samples so it means that every agricultural commodity will residual pesticides-free in 70.3%. The detected residual pesticides showed for a total of 69 cases (29.7%). Two of samples violate Korean MRL (0.9%). The ratio of EDI compared to ADI resulted in only from 0.00087 to 0.902%. In result, we can assume that all detected residual pesticides are very safe level and current policies of Korean pesticides control may be working.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.22-29
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• 2019

Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

• The Korean Journal of Pesticide Science
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• v.17 no.2
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• pp.77-83
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• 2013

This study was performed to investigate pre-harvest residue limit (PHRL) in amaranth, to estimate biological half-life of emamectin benzoate and identify the characteristics of the residue. Pesticides of standard and double appplication rate, were sprayed once on amaranth at 0, 1, 2, 3, 5, 7, 10, 14 days before harvest. Amaranth sample was extracted with acetonitrile and partitioned with dichloromethane, and pesticide residues were determined with LC/MS/MS. The limit of detection of emamectin benzoate was 0.01 mg/kg. Recoveries of emamectin benzoate ($B_{1a}$, $B_{1b}$) at two fortification levels of 0.1 and 0.5 mg/kg, $B_{1a}$ were $93.3{\pm}0.7%$ and $93.2{\pm}7.7%$, $B_{1b}$ were $106.6{\pm}1.9%$ and $80.5{\pm}6.6%$, respectively. The biological half-lives of emamectin benzoate were about 2.0 days at standard application rate and 1.7 days at double application rate, respectively. The PHRL of emamectin benzoate were recommended as 0.84 mg/kg for 10 days before harvest.

• Journal of Food Hygiene and Safety
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• v.34 no.5
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• pp.421-430
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• 2019

In this study, 195 pesticide residues in fruit samples (n=150) at local markets in Chungcheongnam-do Chungnam, Korea were monitored using a multi-residue method combined with GC-MS/MS and LCMS/MS. Among 150 fruit samples, 40 types of pesticides were detected in 63 samples and the detection rate was 42.0%. However, the amounts were below the maximum residue limit (MRL). Detection rates for pesticides in each thpe of fruit were as follows ; citrus fruits (55.2%), pome fruits (41.3%), berries (38.7%) and stone fruits (36.0%). Although the sample size was small (n=2), pesticide residues were not detected in tropical fruits. Occurrences of detection of pesticide residues in apple showed the highest level, and mainly, insecticides were detected most frequently. The most commonly detected pesticides residues were bifenthrin (21), pyraclostrobin (17), novaluron (13), boscalid (10), chlorfenapyr (9), trifloxystrobin (9), furathiocarb (9), acetamiprid (8) and chlorpyrifos (8). Five types of residual pesticides (bifenthrin, chlorfenapyr, deltamethrin, fenpropathrin and fenvalerate) were detected in quince, and out of these five, fenpropathrin exceeded the MRL based on the Positive List System (PLS). These results suggested that pesticide residues in fruit samples should be continuously monitored, although residue levels in 63 other fruit samples were evaluated as being within a safe level.

• Food Science and Preservation
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• v.11 no.1
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• pp.57-62
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• 2004

Pesticide contaminants content was determined about both general vegetables marketed at Garak-dong market and organic vegetables cultivated at Hongchun, Kangwon-do. The vegetables were kale, Angelica Keiskei Koidz, celery, lettuce and Allium fistulosum. Pesticide contaminants content of 5 kinds general vegetables were 93.5, 57.7, 112.4, 76.5, 65.2 ppm, respectively. This residual levels were showed 75.35, 70.68, 78.49, 70.49％ about standard level, respectively. Angelica Keiskei Koidz was not able to calculate the residual level because the standard level was not established in Korea. In contrast, the residual levels of organic vegetables were determined 36.4, 21.0, 42.9, 29.1, 25.1ppm, respectively. This level was about 30％ of standard level, 38.93, 36.40, 38.17, 38.04, 38.50％ of general vegetables. At the result, pesticide contaminants content of organic vegetables was less than 40％ of general vegetables.

• The Korean Journal of Pesticide Science
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• v.18 no.3
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• pp.130-140
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• 2014

Recently, some of the previous studies reported that tolclofos-methyl is still exist in ginseng cultivated soil, even though it is has been banned for ginseng. Therefore, the current study was aimed to examine the levels of absorption and translocation of tolclofos-methyl from ginseng cultivated soil to ginseng root and leaf stem for the period of 1 year. For this study, ginseng plants were transplanted in pots and treated with $5.0mg\;kg^{-1}$ of tolclofos-methyl (50% WP). At the end of each interval periods (every three months) the samples (soil, roots and leaf stems) were collected and analyzed the absorption and translocation levels of tolclofos-methyl using gas chromatography and mass spectrometry (GC-MS). The limit of quantitation of tolclofos-methyl was found to be $0.02mg\;kg^{-1}$ and 70.0~120.0% recovery was obtained with coefficient of variation of less than 10% regardless of sample types. In this study, a considerable amount of translocation of tolclofos-methyl residues were found in soil (4.28 to $0.06mg\;kg^{-1}$), root (7.09 to $1.54mg\;kg^{-1}$) and leaf stem (0.79 to $0.69mg\;kg^{-1}$). The results show that the tolclofos-methyl was absorbted and translocated from ginseng cultivated soil to ginseng root and ginseng leaf stem and found to be decreased time-coursely. Secondly, we were also analyzed soil, root and leaf stems samples from Hongcheon, Cheorwon, Punggi and Geumsan by GC-MS/MS (172 pesticides), LC-MS/MS (74 pesticides). In this study, 43 different pesticides were detected ($0.01{\sim}7.56mg\;kg^{-1}$) in soil, root and leaf stem. Further, tolclofos-methyl was detected 4 times separately in root sample alone which is less ($0.01{\sim}0.05mg\;kg^{-1}$) than their maximum residual limit (MRL) in ginseng. Consequently, the results from both studies indicate the residues of tolclofos-methyl found in ginseng cultivated soil and ginseng ensuring their safety level. Moreover, long-term evaluations are needed in order to protect the soil as well as ginseng free from tolclofos-methyl residues.

• Journal of Food Hygiene and Safety
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• v.2 no.1
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• pp.3-8
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• 1987

ABSTRACT-Agricultural products collected from the suburbs of Chuncheon in 1984 were analyzed for carbamate pesticides by GLC-NPD. O-tert-butyl phenyl methyl carbamate(BPMC) was detected in most samples and their residue levels in strawberry, tomato, cucumber, grape, apple and chinese cabbage were in the range of non-detectable to 0.2356 ppm(Av. 0.0539 ppm). 1- naphthyl methyl carbamate(N AC) were detected in cucumber, grape and chinese cabbage and their residue levels were in the range of non-detectable to 0.0265 ppm. O-cumeryl methyl carbamate(MIPC) was detected in only chinese cabbage and its residue levels were in the range of non-detectable to 0.0059 ppm. Detection frequencies of BPMC, MIPC and NAC in the chinese cabbage were higher than those the others.others.

• Horticultural Science & Technology
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• v.34 no.4
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• pp.644-654
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• 2016

Supervised residue trials for mandipropamid in Korean cabbage(Brassica campestris L.) were conducted to establish its pre-harvest residue limit (PHRL), a criterion to ensure the safety of the terminal pesticide residue during cabbage production. Tissues of Korean cabbage were collected at 0, 1, 3, 5, 7, and 10 days after mandipropamid application and subjected to residue analysis. The analytical method was validated by recoveries ranging from 88.2-92.2% at two levels (0.4 and $2.0mg{\cdot}kg^{-1}$), and a limit of quantitation (LOQ) of $0.04mg{\cdot}kg^{-1}$. Mandipropamid residues in Korean cabbage gradually decreased over time. The dissipation rate of the residue would be affected by intrinsic degradation of the compound along with dilution resulting from the fast growth of Korean cabbage. The decay pattern was well fitted by simple first-order kinetics. Biological half-lives of mandipropamid in Korean cabbage ranged from 3.9-4.0 days in two field conditions. Calculated by the regression curve of mandipropamid dissipation, the PHRLs of mandipropamid in Korean cabbage were recommended as 11.07-12.19 and $5.76-6.05mg{\cdot}kg^{-1}$ for 10 and 5 days prior to harvest, respectively.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.502-506
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• 2011

Most countries have the legislation and regulation for POPs control in food. In here, we studied the quantitative analysis of 24 organochlorine POPs (${\alpha}$-HCH 1, ${\beta}$-HCH 2, ${\gamma}$-HCH 3, ${\delta}$-HCH 4, trans-chlrodane 5, 2,4'-DDE 6, ${\alpha}$-endosulfan 7, cis-chlordane 8, 2,4'-DDD 9, endrin 10, ${\beta}$-endosulfan 11, 2,4'-DDT 12, endosulfan sulfate 13, HCB 14, aldrin 15, trans-nonachlor 16, 4,4'-DDE 17, dieldrin 18, 4,4'-DDD 19, cis-nonachlor 20, 4,4'-DDT 21, heptachlor 22, heptachlor epoxide 23 and mirex 24) with GC-ECD. The retention time of analytes were ranged between 19.18 min and 34.69 min, and their peak intervals were over 0.05 min at least. LOQs were ranged 0.003 ~ 0.033 ng/g, and their recovery rates were showed 60.9 ~ 120.8% on the 0.1 ng/g concentration of 24 organochlorine POPs. All tested 30 sundried salts were collected on Korean retailed market, and any analyte was not found in all the samples on LOQ levels.