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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.
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.
Determination of Paraquat in Garlic by LC-MS/MS
ChaeUk Lim,Hyejin Park,unJoo Baek,Jimin Yoon,Juryeong Lee,Byeung Gon Shin,Soon-Kil Cho,Sung-Hee Hong 한국농약과학회 2021 한국농약과학회 학술발표대회 논문집 Vol.2021 No.11
A fast, sensitive, reliable and economical method was developed for the determination of paraquat (a widely used herbicide) in garlic using iquid chromatography-tandem mass spectrometry (LC-MS/MS). Garlic contains numerous sulfur compounds and strong matrix effect that are difficult to analyze in a single run using HPLC. The sample was extracted with 0.1M HCl under heating. Chromatographic separation of paraquat was achieved on a hydrophilic interaction liquid chromatography column (2.1×50mm, 2.7μm) with a gradient program using 50 mM ammonium formate, 0.5% formic acid and acetonitrile as mobile phase. The low salt concentration used in the eluting buffer ensured extended LC-MS analysis of paraquat in garlic without the necessity of frequent source cleaning. The validity of the developed method was evaluated by spiking paraquat in garlic at 0.01 and 0.1mg/kg. Recovery ranged from 76.5 to 100.0%. The limit of detection is < 0.01mg/kg.
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.
Determination of acibenzolar-S-methyl and acibenzolar acid in agricultural commodities by LC-MS/MS
Hyejin Park,ChaeUk Lim,EunJoo Baek,Jimin Yoon,Juryeong Lee,Yong-Kyoung Kim,Sujeong Shin,Hyerim Yu,Byeung Gon Shin,Soon-Kil Cho,Sung-Hee Hong 한국농약과학회 2021 한국농약과학회 학술발표대회 논문집 Vol.2021 No.11
Acibenzolar-s-methyl is a well-known plant activator and fungicide, which is synthetic analog of salicylic acid. Usually, it is not directly toxic to fungi but works by inducing systemic acquired resistance, the natural defence system of plants. The residue definition set in MRL regulation for all agricultural commodities is the sum of acibenzolar-Smethyl(ester form) and acibenzolar acid, expressed as acibenzolar-S-methyl. The current official analytical method(MFDS Food Code) is to hydrolyze acibenzolar-S-methyl in a sample with acibenzolar acid and analyze it with LC-UVD. In this study, a method based on QuEChERS and LC-MS/MS was developed for the simultaneous determination of acibenzolar-S-methyl and acibenzolar acid in agricultural commodities. Two compounds were extracted from matrix with acetonitrile containing 1% formic acid and treated with QuEChERS original salts. Recovery experiments were conducted on 3 agricultural commodities(rice, mandarin, and pepper) and main performance parameters investigated were linearity, recovery, relative standard deviation(RSD), and limit of quantitation(LOQ). The recoveries were within 71.1∼116.9% with the RSD of 0.7∼14.8% and the LOQ of methods were below 0.01mg/kg, and the coefficient of determination (R2) of matrix-matched standards were > 0.995. The proposed method was reproducible and sensitive enough to determine the residues of acibenzolar-S-methyl and acibenzolar acid in agricultural commodities.
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.