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조순길 ( Soon-kil Cho ),이미진 ( Mi-jin Lee ),이정민 ( Jeong-min Lee ),김호진 ( Ho-jin Kim ),박수민 ( Soo-min Park ),박혜진 ( Hye-jin Park ),이승화 ( Seung-hwa Lee ),안종성 ( Jong-sung Ahn ) 한국환경농학회 2018 한국환경농학회 학술대회집 Vol.2018 No.-
2017년 유럽에서 피프로닐에 오염된 계란이 유통된데 이어 국내에서 생산된 일부 계란에서도 살충제가 검출되었다. 피프로닐은 진드기 방제 목적으로 사용되는 살충제로 sulfide, sulfone, amide, sulfoxide의 대사산물을 생성한다. 피프로닐은 물에 1.9 mg/L 정도 용해되고, 아세톤에 545.9g/L가 용해되는 성질이 있어 시료 채취시 아세톤을 사용한다. 농장시설 등에 부착된 피프로닐을 제거하기 위해 5% 탄산나트륨(Na2CO3)과 15% 과산화수소(H2O2)를 권장하고 있다. 이는 피프로닐을 피프로닐설폰으로 산화시킨 다음 반복적으로 사용하여 제거한다. 이러한 제거 작업을 통해 피프로닐이 제거된 정도를 조사할 필요가 있고, 이를 위한 분석법 정립이 필요하다. 시료를 250 mL 용기에 넣고 1% 함유 아세토니트릴 100 mL을 주가하여 10분간 격렬하게 진탕한 후, 3500 rpm으로 원심분리를 하였다. 추출액 1 mL을 0.2 um 멤브레인필터로 여과하여 시험용액으로 하였다. 칼럼은 C18(2.0 mm I.d×50mm, 3 um)을 사용하였고, 이동상은 0.1% 포름산 함유 메탄올과 0.1% 포름산 및 5 mM 아세트산암모늄이 함유된 물을 사용하였다. 분석조건으로 피프로닐의 선구이온은 437 m/z, 생성이온은 368, 255, 290 m/z, positive 조건으로 분석하였고, 피프로닐 설폰의 선구이온은 451 m/z, 생성이온은 415, 282, 244 m/z negative 조건으로 분석하였다. 분석법의 정량한계는 피프로닐 0.92 ug/kg, 피프로닐설폰 0.70 ug/kg이었다. 피프로닐과 피프로닐 설폰을 각각 1, 5, 10, 50, 100 ug/kg 수준으로 검량선을 작성한 결과, r2는 모두 0.9999이었다. 10 ug/kg과 50 ug/kg 수준의 3반복 회수율 실험결과, 10ug/kg 수준에서 피프로닐은 74.7±0.56%, 피프로닐 설폰은 88.9± 0.27%로 나타났다. 50 ug/kg 수준에서는 피프로닐은 78.6±0.11%, 피프로닐 설폰은 95.2±0.02%로 유효회수율 범위(70~120%)에 포함되었다. 머무름 시간은 피프로닐 5.3 mim, 피프로닐 설폰은 5.7min에서 검출되었다. 교차확인 목적으로 LC/MS/MS로 분석한 시료를 GC/μ-ECD로 분석을 하였다. 분석조건은 주입구 온도 250℃, (5%-Phenyl)-methylpolysiloxane이 충진된 30 m×0.25 mm×0.25 um길이의 칼럼이다. 오븐온도는 130℃에서 300℃까지 승온 조건으로 분석하였고, 머무름시간은 피프로닐 11.64 min, 피프로닐 설폰12.79 min으로 LC/MS/MS와 GC/μ-ECD 모두 표준물질과 시료의 결과가 일치함을 알 수 있었다. 정립된 분석법은 피프로닐 오염도조사를 위한 분석법으로 활용할 수 있을 것으로 판단된다.
퀘쳐스 전처리와 질량분석기를 이용한 과일봉지와 버섯배지 중 463종 다성분 분석법 정립 및 검증
박혜진 ( Hyejin Park ),임채욱 ( Chaiuk Lim ),백은주 ( Eunjoo Baek ),신병곤 ( Byeung Gon Shin ),조순길 ( Soon-kil Cho ),홍성희 ( Sung-hee Hong ) 한국환경농학회 2022 한국환경농학회 학술대회집 Vol.2022 No.-
For the safety management of agricultural products, proper management of the cultivation environment such as agricultural materials(e.g. fruit bags, mushroom culture media, and so on), soils, and agricultural water must be preceded. It is necessary to establish analytical method to accurately and reliably analyze residual pesticides in the cultivation environment. In this study, a QuEChERS method for simultaneous determination of 463 pesticide residues in fruit bags and mushroom culture media was developed and validated. The samples were initially extracted with acetonitrile using of partitioning salts composed trisodiumcitrate dihydrate, disodium hydrogencitrate sesquinhydrate, NaCl, and MgSO<sub>4</sub>. And then targeted pesticides were purified following the dispersive solid phase extraction(d-SPE, PSA) cleanup method and detected by liquid and gas chromatography-tandem mass spectrometry(LC-MS/MS and GC-MS/MS). To evaluate performance of the method, validation experiments were carried out on fruit bags and mushroom culture media at three spiking levels (0.01, 0.05, 0.1 mg kg<sup>-1</sup>). The recoveries of the fruit bags ranged between 70.3 and 120.0% with associated relative standard deviations(RSD) less than 22% for the 458 pesticides. The recoveries of the mushroom culture media ranged between 70.5 and 120.0% with associated relative standard deviations(RSD) less than 22% for the 453 pesticides. The limit of quantification (LOQ) of methods were below 0.01 mg/kg<sup>-1</sup>, and the coefficient of determination (R<sup>2</sup>) of matrix-matched standards were > 0.997. In order for the developed method to be certified as an analytical method determined by the head of NAQs, cross-validation of the three labs is in progress.
질량분석기를 이용한 농산물 중의 Acetochlor 대사산물, EMA와 HEMA의 정량
임채욱 ( Chaiuk Lim ),박혜진 ( Hyejin Park ),백은주 ( Eunjoo Baek ),윤지민 ( Jimin Yoon ),이주령 ( Juryeong Lee ),신병곤 ( Byeung Gon Shin ),조순길 ( Soon-kil Cho ) 한국환경농학회 2021 한국환경농학회 학술대회집 Vol.2021 No.-
Acetochlor is a selective herbicide that controls a broad spectrum of annual grasses, sedge, and broadleaf weeds primarily in corn. MRLs are established for the combined residues of acetochlor and its ethyl methyl aniline-(EMA) and hydroxyethyl methyl aniline-(HEMA) producing metabolites, expressed as acetochlor equivalents. A fast and simple quantitative method for analysis of metabolites of acetochlor, EMA and HEMA in agricultural products has been developed. EMA was determined by gas chromatography tandem mass spectrometry and HEMA by liquid chromatography tandem mass spectrometry. Two compounds were extracted from matrices with acetonitrile containing 1% formic acid and the use of partitioning salts composed of NaCl and MgSO<sub>4</sub> based on QuEChERS method. Recovery experiments were conducted on pepper, brown rice and mandarin. Key performance parameters investigated were linearity, recovery, relative standard deviation(RSD), limit of detection, and limit of quantitation. The recoveries were within 70.6∼106.8% with relative standard deviation (RSD) of 0.7∼7.3% and the limit of quantification (LOQ) of methods were below 0.01 mg/kg, and the correlation coefficient (r<sup>2</sup>) of matrix-matched standards were > 0.995.
퀘쳐스 전처리와 LC-MS/MS를 이용한 Thiodicarb와 Methomyl의 정량
박혜진 ( Hyejin Park ),임채욱 ( Chaiuk Lim ),백은주 ( Eunjoo Baek ),윤지민 ( Jimin Yoon ),이주령 ( Juryeong Lee ),신병곤 ( Byeung Gon Shin ),조순길 ( Soon-kil Cho ) 한국환경농학회 2021 한국환경농학회 학술대회집 Vol.2021 No.-
Both methomyl and thiodicarb belong to the group of oxime carbamate insecticides that acts by inhibiting acetylcholinesterase activity. The residue definition set in MRL regulation for all agricultural commodities is the sum of methomyl and thiodicarb, expressed as methomyl. Thiodicarb consists essentially of two methomyl moieties joined through their amino nitrogen by sulfur. Stoichiometry has to be applied to the calculus of the concentration, and the conversion factor of thiodicarb has to be multiplied by two. A Liquid chromatography tandem mass spectrometry was used for the simultaneous determination of thiodicarb and its degradation product methomyl as a total residue of thiodicarb in brown rice. Thiodicarb is known to degraded during analysis; therefore, a through investigation was carried out, revealing that thiodicarb degrades to methomyl immediately after spiking into a matrix of grain product. Two compounds were extracted from brown rice with acetonitrile containing 1% formic acid and the use of partitioning salts composed of NaCl and MgSO<sub>4</sub> based on QuEChERS method. Recovery experiments were conducted on brown rice. Main performance parameters investigated were linearity, recovery, relative standard deviation(RSD), limit of detection, and limit of quantitation. The recoveries were within 72.2∼96.0% with relative standard deviation (RSD) of 0.5∼2.3% and the limit of quantification (LOQ) of methods were below 0.01 mg/kg, and the coefficient of determination (R<sup>2</sup>) of matrix-matched standards were > 0.997.
퀘쳐스 전처리와 질량분석기를 이용한 논과 밭 토양 중 463종 다성분 분석법 정립 및 검증
백은주 ( Eunjoo Baek ),박혜진 ( Hyejin Park ),임채욱 ( Chaiuk Lim ),신병곤 ( Byeung Gon Shin ),조순길 ( Soon-kil Cho ),홍성희 ( Sung-hee Hong ) 한국환경농학회 2022 한국환경농학회 학술대회집 Vol.2022 No.-
Residual pesticides remaining in the soil may be absorbed and transferred to crops, causing unintentional contamination of agricultural products. So, proper management of the cultivation environment such as soils must be preceded. It is necessary to establish an analytical method to accurately and reliably analyze residual pesticides in paddy and unpland soils. In this study, a QuEChERS method for simultaneous determination of 463 pesticide residues in paddy and upland soils was developed and validated. Soil samples were extracted using a modified QuEChERS.. And then targeted pesticides were purified following the dispersive solid phase extraction(d-SPE, PSA) cleanup method and detected by liquid and gas chromatography-tandem mass spectrometry(LC-MS/MS and GC-MS/MS). To evaluate performance of the method, validation experiments were carried out on paddy and unpland soils at three spiking levels (0.01, 0.05, 0.1 mg kg<sup>-1</sup>). The recoveries of the paddy soil ranged between 70.15 and 120.0% with associated relative standard deviations(RSD) less than 22% for the 445 pesticides. The recoveries of the unpland soil ranged between 70.62 and 115.5% with associated relative standard deviations(RSD) less than 22% for the 449 pesticides. The limit of quantification (LOQ) of methods were below 0.01 mg/kg<sup>-1</sup>, and the coefficient of determination (R<sup>2</sup>) of matrix-matched standards were > 0.997. In order for the developed method to be certified as an analytical method determined by the head of NAQs, cross-validation of the three labs is in progress.
질량분석기를 이용한 농산물 중의 Glufosinate의 정량
임채욱 ( Chaiuk Lim ),박혜진 ( Hyejin Park ),백은주 ( Eunjoo Baek ),신병곤 ( Byeung Gon Shin ),조순길 ( Soon-kil Cho ) 한국환경농학회 2022 한국환경농학회 학술대회집 Vol.2022 No.-
Glufosinate is phosphorus-containing ammonium type that is widely used as crop protection for food crops and also in oil palm planations. Due to zwitterionic nature, previously reported methods for determination of glufosinate usually require derivatization. A fast and simple quantitative method for analysis of glufosinate in agricultural products has been developed. Glufosinate was determined by liquid chromatography tandem mass spectrometry and was extracted from matrices with methanol containing 1% formic acid on quick polar pesticides (QuPPe) method. Recovery experiments were conducted on pepper, brown rice and mandarin. Key performance parameters investigated were linearity, recovery, relative standard deviation (RSD), limit of detection, and limit of quantitation. The recoveries were within 76.9∼100.6% with relative standard deviation (RSD) of 2.5∼16.8% and the limit of quantification (LOQ) of methods were below 0.01 mg/kg, and the coefficient of determination (R<sup>2</sup>) of matrix-matched standards were > 0.995. The results obtained demonstrated that the method has achieved the requirements of the criteria for acceptance of single laboratory method validation.