• The Korean Journal of Pesticide Science
• /
• v.19 no.1
• /
• pp.22-31
• /
• 2015

This study was carried out to monitor the current status of pesticide residues in selling agricultural products via online and assessed their safety in 2014. A total of 124 samples were purchased six times from March to August 2014 twenty online shopping malls randomly. These samples were analysed 208 pesticides by multiresidue method using a GC-ECD/NPD and a LC-MS/MS and confirmed by a GC-MSD. As a result of analysis, residual pesticides samples were 11 (8.9%) such as leek, young radish, welsh onion etc, of which 2 samples (1.6%) such as sesame bud (Chlorothalonil), artemisia (Chlorpyrifos) were violated Korea Maximum Residue limits (MRLs). 11 kinds of pesticides (19 times) were detected in 11 samples. Risk assessment evaluated human health exposure with the ratio of EDI (Estimated daily intake) to ADI (Acceptable daily intake) of pesticides detected. %ADI (the ratios of EDI to ADI) were 0.04~95.70% and some samples represented a fairly dangerous levels. In particular, Chlorothalonil in the sesame bud was shown as a significant risk close to 100% of %ADI. Accordingly, it is recommended to strengthen a safety check on agricultural products in online sales.

• Journal of Food Hygiene and Safety
• /
• v.36 no.1
• /
• pp.9-16
• /
• 2021

The monitoring of residual pesticides in dried chili peppers and chili powders, which are circulated in Seoul from 2018 to 2019, was conducted for safety evaluation. As a result of analyzing for 71 kinds of pesticide residues in 101 cases of samples, pesticides were detected in 87 samples; however, no samples exceeded the MRLs (Maximum Residue Limits). Detection rates of pesticides in dried chili peppers and chili powders were 73.3% and 91.5%, respectively. The detection rate of residual pesticides in chili powders was a little higher than that in dried chili peppers. Twelve types of pesticides were detected, however, those pesticides were acceptable to use on peppers, according to the Crop Protection Guidelines. The most frequently detected pesticide was pyraclostrobin followed by flubendiamide, azoxystrobin, and chlorantraniliprole. The risk for detected pesticides was estimated as the ratio of ADI (Acceptable Daily Intake) to food intake rate. The ADI value resulting by intake of dried chili peppers and chili powders was in the range of 5.66E-05 to 3.34E-02, which was within a safe level.

• Korean Journal of Environmental Agriculture
• /
• v.42 no.3
• /
• pp.203-210
• /
• 2023

Ferimzone Z is a fungicide for effectively controlling rice blast. Under light irradiation conditions, it undergoes a rapid conversion to its E-stereoisomer. Given the importance of isomers in risk assessments of residues in crops, an analytical method was developed for individual isomer quantification. A comparative analysis performed using two columns in HPLC-MS/MS demonstrated that the isomers were successfully separated using the Cadenza column. For the brown rice sample preparation, 5 g of the homogenized sample was saturated with 7 mL of water. The sample was then extracted with a 10 mL mixed solvent of acetonitrile and ethyl acetate (1:1, v/v) that contained 0.1% formic acid, and it was subsequently partitioned with magnesium sulfate and sodium chloride. The upper layer was purified using dSPE containing C₁₈ and PSA sorbents. The established method was subjected to method validation, and it showed recovery rates of 90.6-98.8% (RSD ≤ 3.9%) at concentrations of 0.01, 0.1, 2 mg/kg, with a soft matrix effect (%ME) ranging from -3.1% to +6.5%. This method can be employed in monitoring studies of brown rice to determine the conversion ratio from the Z isomers to the E isomers.

• Analytical Science and Technology
• /
• v.19 no.1
• /
• pp.107-114
• /
• 2006

Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

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

• Korean Journal of Food Science and Technology
• /
• v.41 no.5
• /
• pp.483-489
• /
• 2009

Herein, we present the results of our investigation of 61 pesticide residues in 100 samples of green teas obtained from Korean markets. Bifenthrin, chlorpyrifos, dicofol, EPN, chlorfenapyr, tebuconazole, cyhalothrin, difenoconazole, and tebufenpyrad were detected in 22 of the 100 green tea samples. The quantity of pesticide residues for bifenthrin was 0.12 ppm (maximum residue limits (MRLs): 0.3 ppm) in one sample, chlorpyrifos was 0.24-0.78 ppm (MRLs: 2.0 ppm) in three samples, dicofol was 1.64-4.19 ppm (MRLs: 50.0 ppm) in two samples, EPN was 0.13 ppm (MRLs: 0.05 ppm) in one sample, chlorfenapyr was 0.01-1.23 ppm (MRLs: 3.0 ppm) in 16 samples, tebuconazole was 0.71 ppm (MRLs: 5.0 ppm) in one sample, cyhalothrin was 0.05-0.3 ppm (MRLs: 2.0 ppm) in five samples, difenoconazole was 0.23 ppm (MRLs: 2.0 ppm) in one sample, and tebufenpyrad was 0.06-0.07 ppm (MRLs: 2.0 ppm) in two samples. More than two pesticide residues were detected in seven samples. All detected pesticide residues (with the exception of EPN) were within the MRLs.

• Journal of Life Science
• /
• v.22 no.11
• /
• pp.1456-1462
• /
• 2012

Sorafenib is a multikinase inhibitor and an oral anticancer drug approved for the treatment of patients with advanced renal cell carcinoma and those with unresectable hepatocellular carcinoma. The purpose of this study was to develop an efficient method of the determination of sorafenib in human plasma using tandem mass spectrometry coupled with liquid chromatography (LC/MS/MS) and validate the method by the guidelines of the Korean Food and Drug Administration (KFDA). Plasma samples ($100{\mu}l$) were added with chlorantraniliprole as an internal standard and then mixed with the 0.1% formic acid-containing extraction solution composed of isopropyl alcohol and ethyl acetate (1:4, v/v). After centrifugation, the supernatant was concentrated at $45^{\circ}C$ under negative pressure and centrifugal force. The residue was reconstituted with a mobile phase and injected into the HPLC instrument using a reverse phase Waters XTerra$^{TM}$ C18 column (particle size $3.5{\mu}m$). Liquid chromatography was carried out within the run time of 5 min using a mobile phase composed of buffer (0.1% formic acid and 10 mM ammonium formate), methanol, and acetonitrile (1:6:3, v/v/v). The analytes were monitored by tandem mass spectrometry in the multiple reaction monitoring method programmed to detect sorafenib at 'm/z 465.2 ${\rightarrow}$ 252.5' and chlorantraniliprole at 'm/z 484.4 ${\rightarrow}$ 286.2' with positive electrospray ionization mode ($ES^+$). The result showed the proper linearity ($r^2$ > 0.99) over the range of 2,000-5,000 ng/ml with good accuracy (90.7-103.9%) and precision (less than 10%). The newly developed method using LC/MS/MS was validated by the guideline of KFDA and identified as more sensitive compared to the previous methods.

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

• Korean Journal of Environmental Agriculture
• /
• v.38 no.3
• /
• pp.173-184
• /
• 2019

BACKGROUND: This study was carried out to investigate pesticide residues from fifty streams in Korea. Water samples were collected at two times. Thee first sampling was performed from april to may, which was the season for start of pesticide application and the second sampling event was from august to september, which was a period for spraying pesticides multiple times. METHODS AND RESULTS: The 136 pesticide residues were analyzed by LC-MS/MS and GC/ECD. As a result, eleven of the pesticide residues were detected at the first sampling. Twenty eight of the pesticide residues were detected at the second sampling. Seven pesticides were frequently detected from more than 10 water samples. Ecological risk assessment (ERA) was carried out by using residual and toxicological data. Four scenarios were applied for the ERA. Scenario 1 and 2 were performed using LC50 values and mean and maximum concentrations. Scenarios 3 and 4 were conducted by NOEC values and mean and maximum concentrations. CONCLUSION: Frequently detected pesticide residues tended to coincide with the period of preventing pathogen and pest at paddy rice. As a result of ERA, five pesticides (butachlor, carbendazim, carbofuran, chlorantranilprole, and oxadiazon) were assessed to be risks at scenario 4. However, only oxadiazon was assessed to be a risk at scenario 3 for the first sampling. Oxadiazon was not assessed to be a risk at the second sampling. It seems to be temporary phenomenon at the first sampling, because usage of herbicides such as oxadiazon increased from April to march for preventing weeds at paddy fields. However, this study suggested that five pesticides which were assessed to be risks need to be monitored continuously for the residues.

• Journal of Food Hygiene and Safety
• /
• v.35 no.3
• /
• pp.225-233
• /
• 2020

By the standards and specifications for hygiene products, three test methods for formaldehyde are specified for each item type of hygiene product. After derivatization using acetylacetone and 2,4-dinitrophenylhydrazine (2,4-DNPH), formaldehyde is analyzed by spectrophotometer and high-performance liquid chromatography (HPLC). Validation of the three test methods was performed on tissue, diaper lining and waterproof layer, and panty liner products. The results of linearity (R²), limit of detection (LOD), limit of quantification (LOQ), recovery rate (%) and reproducibility (%), showed that all three methods are suitable for analyzing formaldehyde in hygiene products. After derivatization with 2,4-DNPH and cetylacetone, formaldehyde was analyzed at 0, 3, 6, 9, 24 and 48 hours by HPLC. Formaldehyde derivatized with 2,4-DNPH showed no statistically significant change in formaldehyde peak area over time (P>0.05). But, acetylacetone-derivatizated formaldehyde showed a negative correlation coefficient (r) over time (P<0.01). We investigated the residual amounts of formaldehyde in 205 hygiene products distributed in Busan. Among 74 disposable diaper products tested, 73 had low concentrations of formaldehyde (0.13-29.87 mg/kg). Moreover, formaldehyde was not detected in any of 78 tissue, 27 disposable paper towel, 12 disposable dishcloth, 7 paper cup, one brand of paper straw and 6 disposable napkin products.