• The Korean Journal of Pesticide Science
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• v.16 no.1
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• pp.28-34
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• 2012

We analysed 149 samples of Korean traditional herbal tea materials. The 156 pesticides were analyzed by GC/ECD and NPD, detected pesticides were confirmed by GC-TOF/MS. Sample preparation was performed bv multi-residue analysis method of multiclass pesticides of the Korea Food Code. The residual pesticides were detected in 22 samples(14.8%), the highest detection frequency samples are lycium and jujube. Detected pesticides in Korean traditional herbal tea materials were chlorpyrifos (5 samples), chlorothalonil (3 samples), cypermethrin (3 samples), hexaconazol (3 samples) and cyhalothrin(3 samples). The pesticide types detected in Korean traditional herbal tea materials were organophosphorus(29.2%), pyrethroids(16.7%), organochlorines (12.5%) and triazoles(12.5%). The 5 samples(lycium, jujube, chrysanthemum, balloon-flower, milk vetch root) were detected pesticides below MRLs, 2 samples(cornus fruit, cnidium) were detected pesticides unnotificated MRLs.

• 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.

• Journal of Sasang Constitutional Medicine
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• v.22 no.3
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• pp.132-140
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• 2010

1. Objective: To compare the contents and transfer rate of hazardous substances in crude, washing solution, crude after washing, decoction and remnant after boiling. 2. Methods: The heavy metal contents of each step were measured by inductively coupled plasma mass spectrometer (ICP-MS) and mercury analyzer (MA-2). In order to analyze pesticides in each sample we used simultaneous multi-residue analysis of pesticides by GC/ECD, which was followed by GC/MSD analysis to confirm the identity of the detected pesticide in each sample. In addition, the contents of sulfur dioxide (SO2) were performed by Monier-Williams distillation method. 3. Results: 1) Contents (mg/kg) of heavy metals in decoction of all herbal medicine prescriptions were not detected. 2) Transfer rates (%) of heavy metals from crude to remnant were As (83.3%), Cd (100.0%), Pb (182.6%) and Hg (100.0%). 3) Contents (mg/kg) of residual pesticides were not detected. 4) Transfer rate (%) of sulfur dioxide (SO2) from crude to remnant was 44.2%. 4. Conclusion: Our results showed that boiled herbal medicine prescriptions which we take is safe from the hazardous substances.

• Journal of the Korean Society of Food Science and Nutrition
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• v.39 no.6
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• pp.902-908
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• 2010

In 2008, we monitored residual pesticides of 15 agricultural products such as rice, corn, pea, chestnut, mandarin, lemon, onion, pineapple, lettuce, chard, sweet potato stalk, burdock, squash, sweet pepper and mushroom. Agricultural commodities were collected from markets in 22 provinces (Seoul, Busan, Incheon, Daegu, Ulsan, Daejeon, Gwangju, Wonju, Pohang, Gumi, Changwon, Gimhae, Suwon, Seongnam, Bucheon, Goyang, Yongin, Cheongju, Cheonan, Jeonju, Yeosu, and Jeju). Total 48 pesticides were analysed by multi-residue method using GC/MS/MS. We analysed 1,064 samples and 34 samples (3.20%) were detected. Sweet potatostalk, burdock, chestnuts, peas, corn, chard, squash, mushroom and onions were found to be free from pesticide residues. 6 other agricultural products did not exceed MRLs (Maximum Residue Limits) by the Korean Food Code. Chloropyrifos and fenobucarb were particularly prevalent and also they were detected over 10 times in this monitoring. Nonetheless, the exposed quantity of the 7 residual pesticides is to be considered relatively safe, compared with the acceptable daily intake (ADI) of residual pesticides.

• Korean Journal of Environmental Agriculture
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• v.36 no.4
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• pp.269-278
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• 2017

BACKGROUND: The objective of this study was to evaluate screening method of residual multi pesticides in dead birds by Orbitrap high resolution mass spectrometry (HRMS) to identify the cause of death for birds. METHODS AND RESULTS: Extraction and clean-up method of residual pesticides in liver of dead birds was used QuEChERS (Quick Easy Cheap Effective Rugged and Safe) and method validations was conducted using liquid chromatography and gas chroamtography with triple-quadrupole mass spectrometer (LC/MS/MS and GC/MS/MS) Also, we were evaluated screening method for the determination of residual pesticides in liver of dead birds by LC and GC Orbitrap Mass Spectrometry. Results of method validations, Correlation coefficients of the matrix matched calibration curves were >0.978, and the method detection limits (MDLs) and limits of quantitation (LOQ) were 2.8~72.1 ng/g (18.4 ng/g on average) and 9.0~230 ng/g (58.5 ng/g on average). The accuracy ranged from 69.1%to 130% (103% on average), and the precision values were less than 14.8%(3.8%on average). The screening of residual pesticides in liver of dead birds by LC and GC Orbitrap HRMS was detected monocrotophos, carbofuran, carbosulfan, deltametrin, benfuracarb, carbofuran, phosphamidon, prochloraz in investigated samples. CONCLUSION: This results showed that accurate mass were extraction of residual pesticides in dead birds by Orbitrap HRMS. It suggested that this screening method is applicable to the residual pesticide analysis for the cause of death as a main tool.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.319-326
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• 2016

Colistin is a last resort antimicrobial agent against multi-drug resistant Gram-negative bacteria. This study was conducted to develop an analytical method to determine colistin in fish and shrimp. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with acidified 5% methanol (containing 0.5% formic acid). Then, solid phase extraction (SPE) was used for cleanup. Matrix-matched calibration curves were linear over the calibration ranges (0.05-1.2 mg/kg) for all the analytes into blank sample with $r^2$ > 0.99. All the values fulfilled the criteria requested by the Codex guidelines. Average recoveries ranged from 85.9% to 107.9%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was less than 15%. The limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitation (LOQ) was 0.05 mg/kg. This improved method showed higher accuracy and acceptable sensitivity to meet the CAC guideline requirements and is applicable for the analysis of residual colistin (A+B) in fish and shrimp.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.195-201
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• 2012

We tested for pesticide residues in 124 samples of 22 different items of imported fruits circulated in Gyeonggido. Total 218 pesticides were analyzed by multi-residue method using gas chromatography/nitrogen phosphorus detector-electron capture detector (GC/NPD-ECD), time of flight/mass spectrometer (TOF/MS), ultra performance liquid chromatography/photo diode array (UPLC/PDA), high performance liquid chromatography/fluorescence detector (HPLC/FLD) and mass spectrometer (LC/MS/MS). The pesticides were detected in 18 fruits samples, ranging 0.003~0.3 mg/kg and no samples had violative residue. The separation test to 14 sample pesticides detected was conducted to monitor the current status of pesticide residues according to the partial characteristic. The pesticides were detected in 14 peels ranging 0.03~1.5 mg/kg and 2 fleshes in less than detection limits. These results indicate that imported fruits are safe when the human takes normally but even the small amount of pesticides is harmful when the human takes it in a prolonged period. Therefore, the pesticide residual amounts of imported friuts should be constantly monitored for food safety.

• Journal of Food Hygiene and Safety
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• v.38 no.3
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• pp.131-139
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• 2023

In this study, we investigated pesticide residue levels in 535 domestically distributed agricultural products in South Korea using multi-residue analysis. Agricultural products from 13 regions, including Seoul, were pretreated using QuEChERS and d-SPE, and subsequently analyzed using LC-MS/MS and GC-MS/MS. Residual pesticides were detected in 288 (53.8%) out of the 535 samples, including 40 of apples, 40 of peppers, 33 of mandarins, 31 of peaches, and 144 other commodities. Furthermore, one sample of Korean cabbage exceeded the permitted maximum residue limit (MRL), diniconazole (0.18 mg/kg), detected at about twice the MRL. In total, 91 types of residual pesticides were detected, including fungicides (42), insecticides (48), and a nematicide. The most frequently detected pesticides were dinotefuran (91), carbendazim (75), tebuconazole (61), and pyraclostrobin (59). Our results showed that continuous monitoring of agricultural products is necessary.

• The Korea Journal of Herbology
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• v.23 no.4
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• pp.51-58
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• 2008

Objectives: To compare the contents of heavy metals, residual pesticides and sulfur dioxide before/after a decoction. Methods: The heavy metal contents before/after a decoction were measured by Inductively Coupled Plasma Atomic Emission Spectrometer(ICP-AES) and mercury analyzer. In order to analyze pesticides in 5 samples we used simultaneous multi-residue analysis of pesticides by GC/ECD, which was followed by GC/MSD analysis to confirm the identity of the detected pesticide in each sample. In addition, the contents of sulfur dioxide($SO_2$) were performed by Monier-Williams distillation method. Results: 1. The mean values of heavy metal contents(mg/kg) for the samples were as follows: Galgeun-tang(before decoction-Pb; 0.793, Cd; 0.133, As; 0.016 and Hg; 0.005, after decoction-Pb; 0.033, Cd; 0.004, As; 0.002 and Hg; not detected), Gumiganghwal-tang(before decoction-Pb; 0.934, Cd; 0.197, As; 0.046 and Hg; 0.006, after decoction-Pb; 0.062, Cd; 0.007, As; 0.004 and Hg; 0.0001), Sosiho-tang(before decoction-Pb; 0.891, Cd; 0.134, As; 0.091 and Hg; 0.014, after decoction-Pb; 0.036, Cd; 0.002, As; 0.004 and Hg; not detected), Ojuck-san(before decoction-Pb; 0.907, Cd; 0.136, As; 0.084 and Hg; 0.007, after decoction-Pb; 0.074, Cd; 0.007, As; 0.011 and Hg; 0.0005) and Samsoeum(before decoction-Pb; 1.234, Cd; 0.154, As; 0.016 and Hg; 0.007, after decoction-Pb; 0.094, Cd; 0.006, As; 0.002 and Hg; 0.001). 2. Contents(mg/kg) of residual pesticides before/after a decoction in all samples were not detected. 3. Contents(mg/kg) of sulfur dioxide($SO_2$) before a decoction in Galgeun-tang, Gumiganghwal-tang, Sosiho-tang, Ojuck-san and Samsoeum exhibited 1.2, 3.4, 11.1, 12.0 and 5.7, respectively. However, contents of sulfur dioxide after a decoction in all samples were not detected. Conclusions: These results will be used to establish a criterion of heavy metals, residual pesticides and sulfur dioxide.

• The Journal of Korean Medicine
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• v.30 no.4
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• pp.108-117
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• 2009

Objective: To compare the contents of heavy metals, residual pesticides and sulfur dioxide before/after a decoction. Methods: The heavy metal contents before/after a decoction were measured by inductively-coupled plasma atomic emission spectrometer (ICP-AES) and mercury analyzer. In order to analyze pesticides in 5 samples we used simultaneous multi-residue analysis of pesticides by GC/ECD, which was followed by GC/MSD analysis to confirm the identity of the detected pesticide in each sample. In addition, the contents of sulfur dioxide ($SO_2$) were performed by Monier-Williams distillation method. Results: 1. The mean values of heavy metal contents (mg/kg) for the samples were as follows: Sipjeondaebo-tang (before decoction - Pb; 1.163, Cd; 0.257, As; 0.080 and Hg; 0.016, after decoction - Pb; 0.059, Cd; 0.007, As; 0.006 and Hg; 0.0003), Palmul-tang (before decoction - Pb; 1.181, Cd; 0.242, As; 0.152 and Hg; 0.014, after decoction - Pb; 0.067, Cd; 0.008, As; 0.008 and Hg; 0.0003), Sagunja-tang (before decoction - Pb; 1.285, Cd; 0.283, As; 0.063 and Hg; 0.012, after decoction - Pb; 0.047, Cd; 0.009, As; 0.004 and Hg; not detected) and Samul-tang (before decoction - Pb; 1.025, Cd; 0.169, As; 0.099 and Hg; 0.013, after decoction - Pb; 0.065, Cd; 0.007, As; 0.010 and Hg; 0.001). 2. Contents (mg/kg) of residual pesticides before/after a decoction were not detected in any samples. 3. Contents (mg/kg) of sulfur dioxide ($SO_2$) before a decoction in Sipjeondaebo-tang, Palmul-tang, Sagunja-tang and Samul-tang exhibited 5.0, 6.0, 14.0 and 6.9, respectively. However, contents of sulfur dioxide after a decoction were not detected in any samples. Conclusion: These results will be used to establish a criterion for heavy metals, residual pesticides and sulfur dioxide.