• Title, Summary, Keyword: Modified QuEChERS

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Modified QuEChERS Multi-Residue Analysis Method for 61 pesticides in Fruits using with HPLC and GC-ECD/NPD (HPLC 및 GC-ECD/NPD를 이용한 과일 중 61종 농약의 QuEChERS 전처리 다성분 분석법 개발)

  • Lee, Ju-Young;Hong, Su-Myeong;Kim, Taek-Kyum;Min, Zaw Win;Kim, Yang-Hyeon;Song, Kyung-Ae;Kwon, Hye-Yong;Lee, Hee-Dong;Im, Geon-Jae;Kim, Doo-Ho;Kim, Jang-Eok
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.242-256
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    • 2012
  • QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.

Comparison between the liquid-liquid partition method and modified QuEChERS method for the analysis of pesticide residues in beef fat (소지방 중 잔류농약분석을 위한 액-액분배법과 modified QuEChERS법 비교)

  • Kim, Yoen-Joo;Choi, Yoon-Hwa;Shin, Bang-Woo;Lee, Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.34 no.4
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    • pp.429-439
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    • 2011
  • This article described the comparison of a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation and the classical method established by National Veterinary Research and Quarantine Service (NVRQS) for the determination of pesticide residues in livestock products using GC-tandem mass spectrometry. The classical method by NVRQS used liquid-liquid partioning followed by evaporizing. The modified QuEChERS entailed extraction of 2 g sample with 15 ml acetonitrile containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 6 ml of the extract underwent a cleanup step (in a technique known as column-based solid phase extraction) using 400 mg each of $C_{18}$ and primary secondary amine sorbents plus 1,200 mg magnesium sulfate. The quantitation of individual pesticides by both methods was based on tissue standard calibration curves with a correlation coefficient in excess of 0.98 for the 24 pesticides. The detection limits by the classical method were ranged 1.3~5.0 ${\mu}g$/kg, with mean recoveries between 76.2% and 114.3% except aldrin (59.3%) and deltamethrin (63.6%). The detection limits by modified QuEChERS were ranged 0.3~6.2 ${\mu}g$/kg, with mean recoveries between 68.0% and 114.3% except dimethipin (152.6%), chlorfenvinphos (138.1%), 4,4-DDT (61.5%), aldrin (60.4%) and chinomethionate (30.3%).

Multi-residue Pesticide Analysis in Cereal using Modified QuEChERS Samloe Preparation Method (곡물류 중 잔류농약 다성분 분석을 위한 개선된 QuEChERS 시료 정제법의 개발)

  • Yang, In-Cheol;Hong, Su-Myeong;Kwon, Hye-Young;Kim, Taek-Kyum;Kim, Doo-Ho
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.314-334
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    • 2013
  • This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

Residue analysis of spinetoram and spinosad on paprika leaf using the modified QuEChERS pre-treatment methods

  • Kim, Young-Shin;Yang, Jun-Young;Jin, Na-Young;Yu, Yong-Man;Youn, Young-Nam;Lim, Chi-Hwan
    • Korean Journal of Agricultural Science
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    • v.44 no.4
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    • pp.487-494
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    • 2017
  • Spinosad and spinetoram are widely used insecticides for the control of lepidopteran larvae, leaf miners, and thrips; however, they might also have low toxicity toward beneficial insects like bees. Because these pesticides are easily photolyzed by ultraviolet radiation, the QuEChERS method, with its simple pretreatment procedure, is often used for analyzing residues of spinosad and spinetoram. The present study performed a residue analysis using a modified QuEChERS method by pretreating with ammonium salt. The limit of detection (LOD) of the modified method was 0.05 mg/kg and the limit of quantification (LOQ) was 0.25 mg/kg. The coefficient of determination ($R^2$) for the calibration curve was 0.999. Also, we examined any change in the adhesion of spinosad and spinetoram on the plants depending on a spray volume. The adhesion was approximately 70% when the spray volume was increased from 60 L to 120 L per 10 a whereas the adhesion was approximately 37% when the spray volume was increased from 125 L to 250 L. This showed that the amount of adhesion decreased with the higher spray volume. The efficacy result of spinetoram was that over 90% of Frankliniella occidentalis was controlled with the application volume of 125 L per 10 a. Therefore, the result of this study indicates that control of insects is effective and sufficient with a spray volume of 125 L per 10 a in paprika cultivation facilities.

Simultaneous Analysis of Conazole Fungicides in Garlic by Q-TOF Mass Spectrometer Coupled with a Modified QuEChERS Method

  • Bong, Min-Sun;Yang, Si-Young;Lee, Seung-Ho;Seo, Jung-Mi;Kim, In-Seon
    • Korean Journal of Environmental Agriculture
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    • v.30 no.3
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    • pp.323-329
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    • 2011
  • BACKGROUND: The conazoles, difenoconazole, diniconazole, hexaconazole, penconazole and tetraconazole are a large class of synthetic fungicides used extensively for foliage and seed treatments in agricultural crops. The extensive use of conazoles has brought concerns on the potentiality of environmental contamination and toxicity. Thus studies on the development of methods for monitoring the conazoles are required. METHODS AND RESULTS: A modified quick, easy, effective, rugged and safe (QuEChERS) method was involved in sample preparation. Quadrapole time of flight mass spectrometer (Q-TOF MS) in electron spray ionization (ESI) mode was employed to determine conazoles in garlic samples. The limit of detection (LOD) and limit of quantification (LOQ) of conazoles by Q-TOF-MS ranged from 0.001 to 0.002 mg/L and 0.002 to 0.005 mg/L, respectively. Q-TOF-MS analysis exhibited less than 2.6 ppm error of accurate mass measurements for the detection of conazoles spiked at 0.05 mg/L in garlic matrix. Recovery values of conazoles fortified in garlic samples at 0.02, 0.05 and 0.1 mg/L were between 79.2 and 106.2% with a maximum 11.8% of standard deviation. No detectable conazoles were found in the domestic market samples by using the Q-TOF-MS method. CONCLUSION(s): High degree of confirmation for conazoles by accurate mass measurements demonstrated that Q-TOF-MS analysis combined with a QuEChERS method may be applicable to simultaneous determination of conazoles in garlic samples.

The analysis of pesticide residue in leafy vegetables using the modified QuEChERS pre-treatment methods (QuEChERS 시료 처리법을 활용한 엽채류 중 잔류농약분석)

  • Kim, Yang-Hyeon;Hong, Su-Myeong;Son, Kyung-Ae;Lee, Ju-Young;Min, Zaw Win;Kwon, Hye-Young;Kim, Taek-Kyum;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.16 no.2
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    • pp.121-130
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    • 2012
  • In analyzing pesticide residue, LLE (liquid liquid extraction) is generally applied as one of the existing methods, but needed quite a lot of organic solvents and analytical apparatuses for the sample pre-treatment. In addition to its long analysis time and complex analytical processes, it is required to develop a more rapid and efficient method at present. In order to establish an economic and simple pesticide residue analytical method, this study carried out a comparative experiment on the existing analytical method with a new sample pre-treatment method named QuEChERS (quick, easy, cheap, effective, rugged and safe), which extracts and refines pesticide components by directly adding solid powder into the sample. Both the two analytical methods showed favorable values of correlation coefficient ($R^2$ > 0.99) of calibration curves. In terms of the detection limit (identification limit), imidacloprid showed 0.02 mg/kg, while the rest of pesticides showed a level around 0.05 mg/kg. The results of this experiment revealed that the recovery of LLE was 92.8-100.9% and the RSD was below 2.5%. On the other hand, the recovery of QuEChERS was 92.2-101.6% and RSD was below 1.9%. As a result of comparing the amount of pesticide residue by the time between the two analytical methods by using Paired t-Test, there was no significant difference between the two analytical methods as the p-value ranged from 0.3148-0.9890. Considering the results of the two methods, the QuEChERS method had similar recovery, compared to the analytical method using the existing LLE, and the analytical time was shortened by about one fourth of that of the existing method. Moreover, since it excludes the use of harmful organic solvents like dichloromethane during the process of extraction, thus leading to protecting experimenters health and remarkably reducing the amount of disused solvents, it is judged as an echo-friendly and economic analytical method.

A Study on Rapid Residual Analysis of Benzo(a)pyrene in Agricultural Products and Soils (농산물 및 경작지 토양 시료 중 Benzo(a)pyrene 신속잔류분석법 개선 연구)

  • Kim, Hee-Gon;Ham, Hun-Ju;Hong, Kyong-Suk;Shin, Hee-Chang;Hur, Jang Hyun
    • Korean Journal of Environmental Agriculture
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    • v.39 no.1
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    • pp.44-49
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    • 2020
  • BACKGROUND: Benzo(a)pyrene is a highly toxic substance which has been listed as a Group I carcinogen by the International Agency for Research on Cancer. There have been numerous studies by researchers worldwide on benzo(a)pyrene. Soxhlet, ultrasound-assisted, and liquid-liquid extractions have been widely used for the analysis of benzo(a)pyrene. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these disadvantages, we aimed to establish a rapid residual analysis of benzo(a)pyrene content in agricultural products and soil samples. METHODS AND RESULTS: A Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was used as the pretreatment procedure. For rapid residual analysis of benzo(a)pyrene, a modified QuEChERS method were used, and the best codition was demonstrated after various performing instrument analysis. The extraction efficiency of this method was also compared with Soxhlet extraction, the current benzo(a)pyrene extracting method. Although both methods showed high recovery rates, the rapid residual analysis method markedly reduced both the measurement time and solvent usage by approximately 97% and 96%, respectively. CONCLUSION: Based on these results, we suggest the rapid residual analysis method established through this study, faster and more efficient analysis of residual benzo(a)pyrene in major agricultural products such as rice, green and red chili peppers and also soil samples.

The development and validation of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure for the determination of fluoroquinolones residues in chicken muscle using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) method

  • Park, Sunjin;Kim, Hyobi;Choi, Byungkook;Hong, Chung-Oui;Lee, Seon-Young;Jeon, Inhae;Lee, Su-Young;Kwak, Pilhee;Park, Sung-Won;Kim, Yong-Sang;Lee, Kwang-jick
    • Korean Journal of Veterinary Service
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    • v.42 no.4
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    • pp.289-296
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    • 2019
  • A novel rapid procedure with liquid chromatography tandem mass spectrometry (LC-MS/MS) detection has been developed by changing various conditions including sample preparation such as QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology. This work has been involved the optimization and validation of detection method for fluoroquinolones which are widespread used in livestock especially in the chicken. Five grams of homogenized chicken muscle were extracted with QuEChERS EN and acetonitrile containing 5% formic acid and cleaned with anhydrous magnesium sulfate and C18 sorbent. The separation was performed on Acquity UPLC HSS T3 (2.1 mm×100 mm, 1.8 ㎛) column. The mobile phase A and B were composed of water containing 0.1% formic acid and acetonitrile containing 0.1% formic acid, respectively. Flow rate was 0.25 mL/min and column temperate was 40℃. LC-MS/MS with multiple reaction monitoring has been optimized for ten fluoroquinolones (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, marbofloxacin, norfloxacin, ofloxacin, orbifloxacin, pefloxacin and sarafloxacin). The method developed in this study has been presented good linearity with correlation coefficient (R2) of 0.9971~0.9998. LOD and LOQ values ranged from 0.09 to 0.76 ppb and from 0.26 to 2.29 ppb, respectively. The average recoveries were from 77.46 to 111.83% at spiked levels of 10.0 and 20.0 ㎍/kg. Relative standard deviation (%) ranged 1.28~11.90% on intra-day and 3.10~8.38 % on inter-day, respectively. This analysis method was applicable to the livestock residue laboratories and was expected to be satisfactory for the residue surveillance system.

Evaluation of QuEChERS Method for Determination of pesticide Residues Using GC/NPD and GC/ECD (GC/NPD와 GC/ECD를 이용한 잔류농약 정량 분석법으로써의 QuEChERS의 평가)

  • Cho, Tae Hee;Park, Young Hye;Park, Hye Won;Hwang, Lae Hwong;Cho, In Soon;Kim, Min Jung;Kim, Hyun Jeong;Kim, Mu Sang;Chae, Young Zoo
    • The Korean Journal of Pesticide Science
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    • v.17 no.1
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    • pp.65-71
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    • 2013
  • The modified QuEChERS method was evaluated for rapid determination of pesticide residues in spinach by gas chromatography-nitrogen phosphorous detector (NPD) and electron capture detector (ECD). Fifty GC-amenable pesticides which were most frequently detected in monitoring were selected in the current study. Matrix-matched calibration was performed. The detector response for all pesticides was linear with determination coefficients higher than 0.995. LODs for most compounds ranged between 0.001 and 0.1 ug/g, and about 90% of the compounds had LODs of less than 0.05 ug/g. LOQs ranged from 0.001 to 0.32 ug/g, which were well below the MRLs permitted for most of pesticides. In the majority of cases, the recoveries (80-120%) and relative standard deviations (RSDs) (less than 20%) were within acceptable levels except for dichlorvos, propamocarb, chlorothalonil, dichlofluanid, cyhalothrin and fenvalerate. Also, this method which is applied to routine samples showed good results when comparing with traditional multi-residue method.

Investigation of Resiudal Organochlorine Pesticides in Green Perilla (Perilla frutescens var. japonica Hara) Greenhouse Soil and Its Leaves (들깨 생산단지 시설재배지 중 잔류성유기염소계 농약류 잔류량 조사)

  • Lim, Sung-Jin;Oh, Young-Tak;Ro, Jin-Ho;Yang, Ji-Yeon;Choi, Geun-Hyoung;Ryu, Song-Hee;Moon, Byeong-Chul;Park, Byung-Jun
    • The Korean Journal of Pesticide Science
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    • v.20 no.3
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    • pp.221-227
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    • 2016
  • This study was conducted to investigate residual organochlorine pesticides in green house soil and green perilla leaves. Extraction and clean-up method were developed using the modified QuEChERS method for residual organochlorine pesticides (ROCPs) in soil and green perilla leaves. Recovery and limit of quantitation (LOQ) of ROCPs in greenhouse soil and green perilla leaves were 76.3-113.4 and 79.4-107.3%, 0.03-0.24 and $0.33-0.50{\mu}g/kg$, respectively. Detected ROCPs in greenhouse soil were dieldrin and endosulfan sulfate, the residue were 1.6-9.2 and $22.0-87.8{\mu}g/kg$, respectively. But two pesticides in all green perilla leaf samples were not detected. These results showed that ROCPs residue in greenhouse soil was lower than the level of bioaccumulation occurring.