• The Korean Journal of Pesticide Science
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• v.20 no.3
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• pp.211-220
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• 2016

This study was to develop the analytical reference material of green-pepper for multi-residue analysis of pesticides. According to the ISO Guide 35, ISO Guide 13528 and EURL-PT protocol, the homogeneity, stability, assigned value and uncertainty were calculated to assess if it was suitable to be used as the proficiency test or quality control. The values of the within-bottle standard variation ($s_{wb}$) and the between-bottle standard variation ($s_{bb}$) were 1.7~3.7% of assigned value according to the requirement of the ISO guide 35. And, the uncertainty ($u^*{_{bb}}$) due to inhomogeneity was 0.8~1.1% for all pesticides. The storage stabilities of ten-pesticides at various conditions were assessed. For all target pesticides, the slop ($b_1$) values were smaller than the corresponding values of $[t_{0.95,n-2}{\times}s(b_1)]$ specified by the ISO guide 35, indicating that there were no statistically significant decreases in the concentration of the target pesticides when the analytical reference material was stored at room temperature ($20{\sim}30^{\circ}C$) for 7 days, freezing ($-20^{\circ}C$) for 30 days and deep freezer ($-80^{\circ}C$. except for bifenthrin, fenpropathrin) for 245 days. For proficiency test by using it developed by Korea Institute of Toxicology, inter-lab test was performed with eight organization performing the residual pesticide analysis. We found that there were some different results among them. Some were assessed as questionable or unacceptable for two pesticides and one organization didn't analyze the six pesticides. From these results, this green-pepper analytical reference material containing ten-pesticides could be used as a tool for the proficiency test to improve the reliability or consistency for pesticide residue's results.

• Korean Journal of Environmental Agriculture
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• v.34 no.3
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• pp.230-237
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• 2015

BACKGROUND: To identify the sources of inaccuracy in LC/MS/MS methods used in the routine quantitation of small molecules are described and discussed. METHODS AND RESULTS: Various UPLC coupled to triple quadrupole mass spectrometer and time of flight (TOF) were used to identify the potential sources of inaccuracy and inducing the pitfalls of qualification and quntitation during the veterinary drug residue analysis. Some of stable isotope labelled veterinary drugs, which were used as internal standards, presented "cross-talk", regardless of manufactures of mass spectrometer and types of spectrometer. Group of sulfonamides also presented inaccuracy qualification and quantitation due to the multi-residue analytical method with the same fragment ions at the close retention times. CONCLUSION: The phenomena of "cross-talk" occurring between subsequently monitored transition from stable isotope labelled and isotope non-labelled authentic chemical were identified. To prevent errors and achieve more accurate data during the analysis of small molecules by LC/MS/MS SRM method, Followings should be taken care of and kept checking; purity and concentration of stable isotope as an internal standard, prevention of carry-over during the separation in column, minimizing the ion suppression by matrix effect, identification of retention time, precursor ion and product ion, and full knowledge of data processing including smoothing and peak integration.

• Korean Journal of Environmental Agriculture
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• v.41 no.4
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• pp.288-309
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• 2022

BACKGROUND: The objective of this study was to develop a comprehensive and simple method for the simultaneous determination of 59 veterinary drug residues in livestock products for safety management. METHODS AND RESULTS: For sample preparation, we used a modified liquid extraction method, according to which the sample was extracted with 80% acetonitrile followed by incubation at -20℃ for 30 min. After centrifugation, an aliquot of the extract was evaporated to dryness at 40℃ and analyzed using liquid chromatography combined with tandem mass spectrometry. The method was validated at three concentration levels for beef, pork, chicken, egg, and milk in accordance with the Codex Alimentarius Commission/Guidelines 71-2009. Quantitative analysis was performed using a matrix-matched calibration. As a results, at least 52 (77.6%) out of 66 compounds showed the proper method validation results in terms of both recovery of the target compound and coefficient of variation required by Codex guidelines in livestock products. The limit of quantitation of the method ranged from 0.2 to 1119.6 ng g-1 for all matrices. CONCLUSION(S): This method was accurate, effective, and comprehensive for 59 veterinary drugs determination in livestock products, and can be used to investigate veterinary drugs from different chemical families for safety management in livestock products.

• The Korean Journal of Pesticide Science
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• v.20 no.2
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• pp.104-127
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• 2016

A new analytical method has been developed to determine 320 pesticides in apple and rice. The extraction of pesticides was carried out based on QuEChERS sample extraction, and determination was performed using LC-MS/MS and GC-MS/MS. 320 pesticides were selected for experiments. 251 and 110 pesticides among them were analysed by LC-MS/MS and GC-MS/MS, respectively. 41 pesticides of them were analyzed by both GC-MS/MS and LC-MS/MS. Among pesticides analysed by LC, 242 pesticides (96% of total number) in apple and 237 pesticides (94% of total number) in rice showed recoveries in the range of 70~120% with RSD ${\leq}20%$. In case of pesticides analyzed by GC-MS/MS, 103 pesticides (94% of total number) in apple and 83 pesticides (76% of total number) in rice were successfully validated. These results indicated that LC-MS/MS and GC-MS/MS analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in agricultural products.

• Korean Journal of Food Science and Technology
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• v.42 no.6
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• pp.664-675
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• 2010

This survey was carried out to estimate pesticide residue levels in commercial agricultural products in the year 2009. Residues were examined in 16 commodities (rice, foxtail millet, buckwheat, kidney beans, peanuts, sesame, oranges, grapefruit, kiwifruit, spinach, perilla leaves, leeks, garlic stem, garlic, ginger, and oak mushroom) collected from 22 provinces in Korea. Analyses were performed by multi-methods capable of detecting up to 60 pesticides by LC/MS/MS. A total of 510 samples were collected and analyzed. Of the samples, 96.1% contained no detectable pesticide residues. Detectable residues at or below the MRLs were found in 3.5% of the samples. However, in 0.4% of the samples (spinach and leeks), residue (ethaboxam and fluquinconazole) levels exceeded the MRLs. Furthermore, intake assessments of 7 kinds of pesticide residues were carried out, excluding those exceeding the MRLs. The results showed that the ratios of EDI (estimated daily intake) to ADI (acceptable daily intake) were 0.0001-0.0006%, which indicates that the detected pesticide residues were in a safe range. It is concluded that residual pesticides in agricultural products are properly controlled in Korea.

• Journal of Food Hygiene and Safety
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• v.28 no.1
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• pp.13-18
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• 2013

This study was conducted to monitor residual pesticides in ginseng and balloon flower roots and to assess their risk to human health. All of 112 samples consisted of ginseng and balloon roots were purchased from traditional domestic markets and supermarkets in nine provinces of Korea in 2012. Multi-residue analysis of 122 pesticides was conducted and the analysis was performed by gas chromatography-electron capture detector, gas chromatography- nitrogen/phosphorus detector, and high-performance liquid chromatography. Seven pesticides were detected in 12 root samples and the detection rate was 10.7%. The detected twelve root samples were 10 ginseng root samples and 2 balloon root samples. Pesticides detected in root samples were procymidone, kresoxim-methyl, endosulfan, cypermethrin, tralomethrin, tetraconazole and chlorfluazuron. Among them, two pesticides as tetraconazole in a balloon flower root and cypermethrin in a ginseng root exceeded the recommended maximum residue limit set by Korea Food and Drug Administration. Five pesticides detected from 10 root samples were identified as unregistered pesticides in Korea. In order to do risk assessment with Korean medicinal plant consumption, estimated daily intake of residual pesticides were determined and compared to acceptable daily intake, referring to %ADI values. The range of %ADI values was from 0.006% to 0.333%. Taken together, it demonstrates the pesticides found in the two root samples were below the safety margin, indicating no effect on human health.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.271-282
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• 2013

This is the result of pesticide residue monitoring certified Good Agricultural Practice (GAP) by national agricultural cooperative federation (NACF) from 2009 to 2012. NACF evaluated simultaneously 283 pesticide multi-analysis method with GC (ECD, NPD) and HPLC. 6,590 agricultural products were analyzed in this period. As the results 1) detected 20.27% in 2009, 23.42% in 2010, 28.07% in 2011 and finally 31.75% in 2012, respectively. There was the total detected pesticide residue in the agricultural products. The violated ratio of agricultural products were 2.25% in 2009, 1.82% in 2010, 1.67% in 2011 and 3.47% in 2012, respectively. 13 pesticides went over the maximum residue limits (MRLs); carbendazim was the predominant violation. 40 pesticides; endosulfan was the predominant detected pesticide did not registered respectively crops in Korea. Most agricultural products that were under the MRLs met the safety standard, however agricultural products that contain neither registered nor set up MRL any level for example endosulfan in strawberry. Agricultural products that go over the MRLs with permitted pesticides, for example carbendazim in apple, are rejected. Because of these intricacies continual observation and evaluation will be need during GAP agricultural cultivation.

• Journal of Food Hygiene and Safety
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• v.35 no.2
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• pp.109-117
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• 2020

This study aimed to develop an analytical method for determination of 18 dyes in livestock and fishery products by liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The developed method was validated for linearity, accuracy, limit of quantifications (LOQ) and recovery based on the CODEX guideline (CAC/GL-71). Target matrices (beef, pork, chicken, egg, milk, flatfish, eel, and shrimp) were extracted using acetonitrile (containing 1% of acetic acid) and then, purified with C₁₈ and primary secondary amine (PSA). Calibration linearity was obtained (r²>0.98) and LOQs were 0.002 mg/kg in animal products. The recoveries of dyes were ranged from 63 to 112% and relative standard deviations (RSDs, %) were less than 15%. The residues of 18 dyes were investigated in real samples (n=124) collected from retail markets in South Korea. As a result, a total of seven samples showed positive results for target analytes in fish samples. However, there was no violation according to the maximum residue limits set by the Korean Food Code. The proposed method will be used for routine analysis of dye residues in livestock and fishery products.

• Preventive Nutrition and Food Science
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• v.18 no.2
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• pp.145-149
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• 2013

We tested for residual pesticide levels in dried vegetables in Seoul, Korea. A total of 100 samples of 13 different types of agricultural products were analyzed by a gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-${\mu}ECD$), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography- ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze for 253 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 11 samples, of which 2 samples (2.0%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in 6 of 9 analyzed dried pepper leaves and 1 sample exceeded the Korea MRLs. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The estimated daily intakes (EDIs) range from 0.1% of the acceptable daily intake (ADI) for bifenthrin to 8.4% of the ADI for cadusafos. The most critical commodity is cadusafos in chwinamul, contributing 8.4% to the hazard index (HI). This results show that the detected pesticides could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring is recommended.

• Analytical Science and Technology
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• v.21 no.6
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• pp.526-534
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• 2008

To determine the trace level of synthetic and natural hormones in food, the improvement of official analytical method and new development of simultaneous determination of hormones were established. On the basis of developed analytical method, the background level of natural hormones and distribution of residual hormones were monitored in meat. Target hormones were six natural hormones such as estrogens ($17{\beta}$-estradiol, $17{\alpha}$-estradiol, estrone), androgens ($17{\beta}$-testosterone, $17{\alpha}$-testosterone), and gestagens (progesterone) and three synthetic hormones such as DES, zeranol, and taleranol. These hormones were analyzed by gas chromatographymass spectrometry. Newly developed multi-residue analysis method was applied for meat sample which were collected from market in the capital region and monitored the presence of residues of synthetic and natural steroid hormones. No residue of synthetic hormones were detected and endogenous level of progesterone was detected in cattle, pig and liver samples tested.