• Journal of Food Hygiene and Safety
• /
• v.24 no.2
• /
• pp.136-142
• /
• 2009

This study was carried out to investigate the current status of suspected endocrine disrupting pesticides among the agricultural products in northern area of Seoul in 2007. 3,026 samples was analyzed by multiresidue method. Detected Pesticide in 11 cases were procymidone, endosulfan, chlorothalonil, chlorpyrifos, cyermethrin, fenvalerate, hexaconazole, carbendazim, pendimethalin, permethrin, parathion and exceeded 7 cases of endosulfan, procymidone, carbendazim, chlorothalonil, chlorpyrifos, cypermethrin, fenvalerate in the maximum residue limits(MRLs). Procymidone, endosulfan, chlorothalonil and chlorpyrifos comprised up to 80.5% in detected pesticides. Among the 321 cases of detected agricultural products, 287 cases(89.4%) were vegetables, 25 cases (7.8%) were fruits, Others were 9 cases(2.8%).

• The Korean Journal of Pesticide Science
• /
• v.15 no.4
• /
• pp.401-416
• /
• 2011

The recent trend for pesticide residue analysis in food involves fast cleanup and use of mass spectrometry to achieve quantitative and qualitative analysis at the same time. Recently, the QuEChERS (quick, easy, cheap, effective, rugged and safe) multi-reside method has received much attention as a fast extraction and cleanup method of pesticide residue analysis. Therefore, multi-residue analysis of 236 pesticides was tested with the QuEChERS method by concurrent use of PTV-GC/TOFMS (gas chromatography/ time-of-flight mass spectrometry with programmable temperature vaporizer). PTV condition was optimized and when the method was applied to apples, pesticide recovery rates (spiked at 400 ng/g) ranged from 80% to 120%, and RSD values were under 10% for most compounds. The results showed that the QuEChERS sample preparation and PTV-GC/TOFMS analysis can be applied to multi-residue analysis of pesticides in fruits and vegetables.

• Journal of Food Hygiene and Safety
• /
• v.24 no.1
• /
• pp.27-37
• /
• 2009

In an effort to evaluate the currents in pesticide residues, 3,020 agricultural products were tested by multiresidue method with 260 pesticides, obtained from the circulation market of in the Gangbuk province in 2007.20.4%(616/3020) of the products were determined to contain pesticides residues, but only 4.1%(124/3020) of these were deemed to be unsuitable by the korea Food Code. Unsuitably products were spinach(21.0%), perilla leaf(17.3%), ulgari(13.6%), leek(12.4%), crowndaisy(12.4%), asterscaber(12.4%), chard(11.1%). Detected pesticides were procymidone(3.9%), endosulfan(2.6%), chlorfenapyr(2.2%), bifenthrin(1.3%), cypermethrin(0.7%), metalaxyl(0.9%), azoxystrobin(0.3%) and chlorothalonil(0.7%). Sixty-four pesticides were detected and 11 pesticides were newly detected in 2007. Thirty-one pesticides in agricultural products exceeded their MRLs.

• Journal of Food Hygiene and Safety
• /
• v.24 no.4
• /
• pp.357-367
• /
• 2009

This study was carried out to investigate the current status of pesticide residues in 3,735 agricultural products in the northern area of Seoul from January to December in 2008. 3,735 samples, comprising 119 types of agricultrural products were assessed via a multiresidue method to detect 260 pesticides. Pesticide residues were detected in 19.7% (737 of 3,735 samples), and the rate at which the detected residues violated the maximum residue levels(MRLs) of the Korean Food Code was 3.2% (121 of 3,735 samples). Pesticide residues were detected in 72 spin-aches, 64 peppers, 45 sweet peppers, 40 perilla leaves, 38 korean cabbages and 37 dried agricultural products. The samples that violated the MRLs included 14 perilla leaves, 13 spinaches, 12 leek, 6 lettuces(leaf), 6 chards and 6 gyeojchaes. Procymidone, endosulfan, chlorfenapyr, cypermethrin, bifenthrin, tebuconazole and fenvalerate were all frequently observed. Procymidone, endosulfan, dimethomorph and diniconazole were the pesticides most frequently detected at levels that violated the Korean Food Code MRLs.

• Korean Journal of Environmental Agriculture
• /
• v.30 no.3
• /
• pp.339-345
• /
• 2011

BACKGROUND: Recently in Korea, the import of agricultural products is rising due to the increasing amount of trade. Unregistered pesticides, allidochlor, propachlor, propham, cycloate, diallate and pebulate are widely used as pesticides for rice cultivation in foreign countries, while they are not registered in Korea. Therefore, the residue amount of imported agri-foods should be verified using the proper official analytical method for each of them that has not registered in Korea. METHODS AND RESULTS: This work was conducted to apply the official method of Korea Food & Drug Administration (KFDA) for determining multi class pesticide multiresidues in agricultural commodities. Brown rice and orange which have different characteristics as a matrix were selected as representative samples for residue analysis. The recoveries of cycloate, diallate and pebulate by GC/MS in fortified brown rice and orange with levels of 0.04~0.4 mg/kg were ranged from 82.8% to 110.3%. The quantification limits of three pesticides in brown rice and orange were 0.04 mg/kg. CONCLUSION: As a result, this method can surely be used as an official method for routine analysis of unregistered pesticides in Korea for imported agri-food.

• Korean Journal of Environmental Agriculture
• /
• v.30 no.1
• /
• pp.60-67
• /
• 2011

BACKGROUND: Because dried herbal medicines have many active ingredients, it is not easy to determine the residue amount after extraction, partition and clean up of pesticides from them. Especially, liquid-liquid partition method is consuming many times and solvents. Macroporous diatomaceous earth(MDE) column was used to replace the separatory funnel for liquid-liquid extraction with dichloromethane to analyze the endosulfan and its metabolite. METHODS AND RESULTS: The residue analysis method using MDE column instead of liquid-liquid partition for determining insecticide endosulfan and its metabolite in 4 dried herbal medicines was developed by GC/MS. As a result, the recovery rates of the pesticides in 4 herbal medicines were ranged from 80.3 to 93.5% for ${\alpha}$-endosulfan, from 81.0 to 100.3% for ${\beta}$-endosulfan and from 80.6 to 95.6% for endosulfan sulfate, respectively. The coefficients of variation for triplicate were ranged from 1.1 to 3.4%. CONCLUSION: The improved methods are more ecofriendly, safer, faster and less laborious than conventional method by KFDA.

• Korean Journal of Food Science and Technology
• /
• v.45 no.3
• /
• pp.382-384
• /
• 2013

We evaluated the presence of uniconazole residual pesticide in agricultural products by using multiclass pesticide multiresidue methods. Samples were collected from January to August, 2012. The pesticide was detected in 14 samples among the 3,632 samples tested. Amount of the uniconazole pesticide ranged from 0.098 to 2.2 mg/kg in the 14 samples. This method was described for the simultaneous determination of uniconazole by using gas chromatography with an electron capture detector (GC-ECD) and mass spectrometry (MS). For evaluating the GC-ECD method, uniconazole was spiked into gyeojachae at a level of 0.05, 0.5 mg/kg. The recoveries of uniconazole with the GC-ECD method ranged from 98.9-109.4%. The results indicate that our method of simultaneous analysis is applicable to uniconazole analysis.

• Journal of Food Hygiene and Safety
• /
• v.32 no.6
• /
• pp.493-499
• /
• 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.

• Journal of Food Hygiene and Safety
• /
• v.22 no.4
• /
• pp.370-374
• /
• 2007

An analytical method for the simultaneous determination of four tetracycline (oxytetracycline, tetracycline, chlortetracycline, doxycycline) in egg samples was developed and validated using liquid chromatography with ultraviolet detection. Egg samples were extracted by the liquid-liquid extraction based on acetonitrile. The chromatographic separation was achieved on a reverse phase C8 column with gradient elution using a mobile phase of 20 mM oxalic acid (pH 1.5)/acetonitrile. The procedure was validated according to the Food Drugs Administration guideline determining accuracy, precision, and limit of detection. Mean recovery of tetracyclines from spiked egg samples (50, 100, 200, 400, and $800{\mu}g/kg$) were 78.8-109.3%. Linearity in concentration range of $50-800{\mu}g/kg$ was obtained with the correlation coefficient $(r^2)$ of 0.994-0.999. The intra- and inter-day precision (relative standard deviation; RSD) was between 0.3-12.8 and 0.2-11.7%, respectively. Limit of detection (LOD) and limit of quantification (LOQ) for the investigated tetracyclines were 30 and $50{\mu}g/kg$ depending on egg samples, respectively. This method was reliable, sensitive, economical and suitable for routine monitoring of tetracycline residues in dairy egg.

• Journal of Food Hygiene and Safety
• /
• v.28 no.1
• /
• pp.19-23
• /
• 2013

A simple and rapid method has been developed and validated for simultaneous determination of each macrolides residues (spiramycin, josamycin, tilmicosin, tylosin) in chicken muscle by high-performance liquid chromatography- photo diode array (HPLC-PDA). Chicken muscle sample have been extracted with liquid-liquid extraction process; analytes was extracted by acetonitrile, and then defatted with hexane saturated by acetonitrile. The HPLC separation was performed on a Unison UK-$C_{18}$ ($150mm{\times}3.0mm$, $3{\mu}m$) with a gradient system of 0.1% trifloroacetic acid (TFA) and 0.1% trifloroacetic acid (TFA) in acetonitrile as the mobile phase. The drugs were detected at 232 nm for spiramycin and josamycin, and 287 nm for tilmicosin and tylosin. The limits of quantification (LOQs) were between 27 and $59{\mu}g/kg$; and the intra- and inter-day precision (relative standard deviation; RSD) was between 0.9-13.2 and 2.4-13.1%, respectively in chicken muscle sample. The method may has been successfully applied for multiresidue determination of four macrolides below the maximum residue limits (MRLs) established by the European Union (EU).