• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.161-173
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• 2015

The multiresidue method 4.1.2.2 in Korea Food Code was extended for the analysis of 24 unregistered pesticide residues. The method includes acetonitrile extraction, liquid-liquid partition, Florisil SPE clean-up and GC analysis. The limits of quantification (LOQ) range of the method was 0.02~0.05 mg/kg for orange, brown rice and banana. The linearity for targeted pesticides were $R^2$ > 0.99 at the level ranged from 0.05 to 5 mg/L. Recovery test was performed at two concentration levels of LOQ and 4~10 times of LOQ. Recoveries and relative standard deviations (RSDs) of target pesticides were acceptable, showing 70~120% range and less than 20%, respectively, except for ethiprole, picloram and sulcotrion. This method is effectively applicable to routine analysis of target pesticides in orange, brown rice and banana.

• Korean Journal of Environmental Agriculture
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• v.31 no.2
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• pp.157-163
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• 2012

BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

• Korean Journal of Environmental Agriculture
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• v.33 no.4
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• pp.388-394
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• 2014

BACKGROUND: Aclonifen is used as a systemic and selective herbicide to control a wide spectrum broad-leaf weeds by inhibition carotenoid biosynthesis, and then its MRLs(Maximum Residue Limits) will be determined in onion and garlic. In this study, a new official method was developed for aclonifen determination in agricultural products to routinely inspect the violation of MRL as well as to evaluate the terminal residue level. METHODS AND RESULTS: Aclonifen was extracted from crop samples with acetone and the extract was partitioned with dichloromethane and then purified by silica solid phase extraction(SPE) cartridge. The purified samples were detected GC using an ECD detector. Limits of detection(LOD) was 0.001 mg/kg and quantification(LOQ) was 0.005 mg/kg, respectively. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n=5). The recoveries were ranged from 74.3 to 95.0% with relative standard deviations(RSDs) of less than 8%. All values were consistent with the criteria ranges requested in the Codex guidelines(CAC/GL 40). CONCLUSION: The proposed analytical method was accurate, effective and sensitive for aclonifen determination and it will be used to as an official method in Korea.

• Korean Journal of Environmental Agriculture
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• v.32 no.3
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• pp.214-223
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• 2013

BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP; 2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

• 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 Chemical Society
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• v.37 no.6
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• pp.590-598
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• 1993

The simultaneous analysis of samples, 16 organic pesticides in water among 129 priority pollutants listed by EPA, was performed by GC-ECD (electron capture detector) and GC/MS-SIM (selected ion monitoring). Two extraction procedures, liquid-liquid extraction (LLE) and solid-phase extraction (SPE), were studied as an extraction and concentration method. Accuracy and precision of the methods were measured by the calculation of mean recovery and mean relative standard deviation. Finally, the detection limits, the experimental limitations, and prospects were discussed.

• Journal of Food Hygiene and Safety
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• v.37 no.4
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• pp.238-248
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• 2022

This study was conducted to evaluate the safety of 208 types of residue pesticides on 150 dried agricultural products in Ulsan. The pesticide residues were detected using GC-MS/MS, LC-MS/MS, GC/ECD, GC/NPD, and LC/PDA. The detection rate was 19.3% (29 of 150 samples), and 28 types of pesticides were detected. Two of the 29 pesticide residues exceeded the maximum residue limit (MRL). Difenoconazole was detected in Ulleungdo aster, and chlorothalonil and chlorpyrifos were detected in chili pepper leaves. In the vegetable group, the frequency of pesticide residues was found to be the highest in dried leafy vegetables, followed by dried fruiting vegetables other than cucurbit vegetables, and then dried stalk and stem vegetables. The pesticide types detected in the commercial dried agricultural products were fungicide (60%), insecticide (23.8%), and acaricide (16.3%). In the validation study, the values of limit of detection (LOD), limit of quantitation (LOQ), coefficient of determination (R²), and recovery rate were in the range of 0.0001-0.0409 mg/kg, 0.0003-0.1241 mg/kg, 0.994-0.999, and 81.58-116.79%, respectively. The ratio of estimated daily intake (EDI)/acceptable daily intake (ADI) was 0.00002-0.31395%.

• 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.32 no.6
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• pp.493-499
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• 2017

This study was conducted to monitor the current status of pesticide residues and sulfur dioxide in a total of 91 functional rice products from February to October 2016. Multi class pesticide multiresidue methods of 220 pesticides was performed by the GC/ECD, GC/NPD, GC/TOF/MS, LC/PDA, and LC/FLD. As a result of analysis, the pesticides were detected in 3 samples, representing a detection rate of 3.3%. The kind of pesticides was propiconazole and isoprothiolane used for germicide in agriculture or plant growth regulator purposes. The detected levels were 0.0340~0.0566 mg/kg, which were under the MRL (Maximum Residues Limits). The contents of sulfur dioxide in 91 samples by the Monier-Williams method were not detected. Risk assessment of pesticides evaluated using human health exposure with the ratio of EDI (Estimated daily intake) to ADI (Acceptable daily intake). %ADI (the ratios of EDI to ADI) were 0.24~1.25% with safety level.

• Korean Journal of Environmental Agriculture
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• v.38 no.3
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• pp.205-212
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• 2019

BACKGROUND: This survey conducted on agricultural products in Incheon for the past three years from 2016 to 2018 to detect residual pesticides and to monitor the use of pesticides. METHODS AND RESULTS: Residual pesticides were analyzed for a total of 5,937 agricultural products in Samsan wholesale market, traditional market and large retailers in Incheon. Samples were analyzed by multi class pesticide method using GC-MS/MS, LC-MS/MS, GC-ECD/NPD, and UHPLC. In 59 cases (1.0%) residual pesticides were detected improperly and these cases exceeded maximum residue limits (MRLs). CONCLUSION: The ratios of violative agricultural products were similar each year at approximately 1.0% per year, but the residual pesticide detection rates with the limit included in the samples were shown to be gradually decreasing to 17.9%, 12.6%, and 11.2% annually. The frequency of violative residual pesticides was high in order of Diazinon, Chlorpyrifos, Iprodione, etc. Residual pesticide monitoring might be needed in the future continuously, as violations in agricultural products distributed in Incheon are shown at a similar level every year.