A method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for neonicotinoid pesticide analysis in agricultural products. Four compounds (imidacloprid, clothianidin, acetamiprid, thiacloprid) were extracted with acetonitrile from agricultural products and cleaned up by NH2 solid-phase extraction procedure, and eluted with 0.1% formic acid in methanol/dichloromethane (5/95, v/v). The limit of detection and quantification were 0.0001-0.0005 mg/kg and 0.001 mg/kg, respectively. The mean recoveries of neonicotinoid pesticide from agricultural products were in the range of 90.7-100.9% and 94.4-99.8%, as spiked at 0.2 mg/kg and 0.02 mg/kg, respectively. This validation satisfied the national criteria for pesticide analytical methods. In summary, The present method is fast, precise and sensitive enough for the Positive List System (PLS), and we conclude that the method is also suitable for neonicotinoid pesticide determination in a wide range of agricultural products.

LC-MS/MS를 이용하여 신속하고 정밀한 카벤다짐 분석법을 연구하였다. 농산물 중 카벤다짐은 acetonitrile로 추 출한 후 SPE cartridge을 이용하여 전처리를 수행하였으며, 최소 검출한계 및 정량한계는 각각 0.001과 0.004 mg/kg 이었다. 농산물에 각각 1.0 mg/kg 및 0.02 mg/kg 농도의 카벤다짐을 첨가하여 분석 시 회수율과 정밀성은 각각 상추 가 84.9%, 1.0% 및 87.8%, 3.8% 얼갈이배추가 83.4%, 1.5% 및 86.8%, 2.7% 양배추가 86.4%, 2.0% 및 77.3%, 1.5% 근대가 83.3%, 0.2% 및 86.8%, 2.0 % 이었으며, 콩 나물은 85.9%, 3.0% 및 90.1%, 1.3%, 그리고 숙주나물이 83.3%, 2.0% 및 85.9%, 1.9% 로 조사되었다. 본 연구의 시험법은 식품공전의 다성분분석법에 비해 신속하고 정밀 한 분석법으로 농산물에 대한 카벤다짐 분석에 적합한 것으로 조사되었다.

Pesticide residues were investigated in 16 commodities (rice, foxtail millet, buckwheat, kidney bean, peanut, sesame, orange, grapefruit, kiwifruit, spinach, perilla leaves, leek, garlic stem, garlic, ginger and oak mushroom)collected from 22 provinces (Seoul, Busan, Incheon, Daegu, Daejeon, Gwangju, Ulsan, Suwon, Seongnam, Goyang,Bucheon, Yongin, Cheongju, Jeonju, Jeju, Cheonan, Changwon, Pohang, Gumi, Jinju, Wonju and Yeosu) in 2009. Pesticides (172 kinds) were analyzed using multiresidue method by GC/MS/MS from 510 samples, and phenthoate in kiwifruit was violated by exceeding MRL. The intake assessment for 24 kinds of pesticide residues including the detected pesticides at multi pesticide residue monitoring (bifenthrin etc.) were carried out. The result showed that the ratio of EDI (estimated daily intake) to ADI (acceptable daily intake) was 0.000007~0.458% which means that the detected pesticide residues were in a safe range so that residual pesticides in the agricultural products in Korea.

This study was carried out to investigate the current status of pesticide residues in 3,988 agricultural products in the northern area of Seoul from January to December in 2009. 3,988 samples comprising 109 types of agricultural products were assessed via a multiresidue method to detect 272 pesticides. Pesticide residues were detected in 25.6% (1,021 of 3,988 samples), and the rate at which the detected residues violated the maximum residue levels (MRLs) of the Korean Food Code was 2.2% (89 of 3,988 samples). The agricultural products which exceeded their maximum residue limits were leek, ginseng, welsh onion, crown daisy and lettuce (leaf). Additionally, the most frequently detected pesticide that exceeded the regulation maximum was endosulfan, procymidone, tolclofos-methyl,iprodione and flutolanil.

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 spinaches, 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.

The content of residual pesticides in commercial agricultural products in Gyeongsangbuk-Do area was investigated for 5 years extending the year 2004 through 2008. The detection rates of residual pesticides in agricultural products by year were similar in range of 11.6~16.4%. But the violation rates showed lower values in the last years from 4.5% of the year 2004 to 0% of the year 2007. The highest residual concentration of each pesticide detected in commercial agricultural products was investigated by year. That is, in the year 2004 and 2005, chlorpyrifos, chlorothalonil, diazinon, endosulfan, ethoprophos, fenarimol and procymidone were detected over the tolerance in kale, parsley, celery, chard and lettuce, and in the year 2006, permethrin in the soybean and peanut. The detection rate and violation rate of pesticides were highly increased in the order of the endosulfan, chlorpyrifos, procymidone, chlorfenapyr, fenitrothion, imazalil, isoprothiolane, methidathion and permethrin. The detection rate and violation rate of pesticides were increased after August every year.

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%).

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.