[논문]Development of Fast Screening Method for Crop Protection Agents in Tobacco by Stir Bar Sorptive Extraction and Thermal Desorption coupled to GC/MS

Min, Hye-Jeong; Lee, Jeong-Min; Shin, Han-Jae; Lee, Moon-Yong; Jang, Gi-Chul

Development of Fast Screening Method for Crop Protection Agents in Tobacco by Stir Bar Sorptive Extraction and Thermal Desorption coupled to GC/MS 원문보기

한국연초학회지 = Journal of the Korean society of tobacco science, v.36 no.1, 2014년, pp.26 - 33

Min, Hye-Jeong (KT&G R&D Headquarters) , Lee, Jeong-Min (KT&G R&D Headquarters) , Shin, Han-Jae (KT&G R&D Headquarters) , Lee, Moon-Yong (KT&G R&D Headquarters) , Jang, Gi-Chul (KT&G R&D Headquarters)

Abstract ▼ AI-Helper

Simultaneous determination of crop protection agents(CPAs) in food are done with multi-residue methods, which are composed of sample clean-up, concentration, chromatographic separation and detection. Stir Bar Sorptive Extraction(SBSE) technique is used for sample preparation of various analytes in several fields. The aim of this study was to develop a sensitive and fast method based on SBSE followed by thermal desorption - gas chromatography - mass spectrometry(TD - GC/MS) to determine CPAs in tobacco sample. For the analysis of tobacco sample prior to the SBSE method, solvent extraction or ultrasound-assisted solvent extraction was performed. methanol was used as the extraction solvent. The extract was then diluted with water. Finally, the sample was subjected to SBSE. A method for fast screening of crop protection agents in tobacco using SBSE-TD - GC/MS has been developed. About 17 CPAs including organochlorine, organophosphorous and others were identified and quantified. This method showed good linearity and high sensitivity for most of the target CPAs. The method was applied to the determination of CPAs at ng/mL levels in tobacco sample. This method is simple, rapid and may be applied in detection of other components.

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문제 정의

This study described a new approach for development of fast screening method for crop protection agents in tobacco by Stir Bar Sorptive Extraction - Thennal Desorption - coupled to GC/MS. The method using SBSE and thermal desorption carried out the extraction and concentration in a single step, and provided enhanced sensitivity for the analytes, as veil as the significant reduction of organic solvents, thus decreasing costs and analytical time.

제안 방법

5 mm PDMS coating layer was used in this study. Extraction efficiency with SBSE was optimized by evaluating the effect of two factors, extraction time and methanol portion. Extraction time was evaluated for different period of time, between 10 and 180 minutes.
In this study, we tried to optimize of stir bar sorptive extraction and thermal desorption coupled to gas chromatography-mass spectrometry for the determination of crop protection agents in tobacco. The optimized methods were applied for determining the CPAs in tobacco, and were evaluated in terms of recovery, linearity and limit of quantification of selected CPAs.
The method using SBSE and thermal desorption carried out the extraction and concentration in a single step, and provided enhanced sensitivity for the analytes, as veil as the significant reduction of organic solvents, thus decreasing costs and analytical time. This method was validated using tobacco samples spiked with 17 CPAs.
agents in tobacco. The optimized methods were applied for determining the CPAs in tobacco, and were evaluated in terms of recovery, linearity and limit of quantification of selected CPAs.
The method using SBSE and thermal desorption carried out the extraction and concentration in a single step, and provided enhanced sensitivity for the analytes, as veil as the significant reduction of organic solvents, thus decreasing costs and analytical time. This method was validated using tobacco samples spiked with 17 CPAs. This method gave good linearity, LOD and LOQ satisfied the requirements of the COREST A GRL.
to the extraction efficiency. To study the influence of extraction time, the equilibrium state between SBSE and target compounds according to extraction time intervals was tested. Effect of extraction time was showed in fig.

대상 데이터

SBSE-TD-GC/MS. Among this compounds, 17 CPAS including organochlorine type(a-BHC, y-BHC, HCB, Alachlor, Heptachlor, Aldrin, Chlorthal dimethyl and Heptachlor epoxide), organophosphorous type(Mevinphos, Chlorpyrifos methyl, Chlorpyrifos ethyl and Bromophos), pyrethroids type(Tefluthrin) and dinitroaniline type(Trifluralin, Benfluralin, Pendim어:halin and Flumetralin) were used in this study.
The commercial stir bar with 30 mm length, 2.5 mm diameter and 0.5 mm PDMS coating layer was used in this study. Extraction efficiency with SBSE was optimized by evaluating the effect of two factors, extraction time and methanol portion.

성능/효과

This method gave good linearity, LOD and LOQ satisfied the requirements of the COREST A GRL. Recoveries of the selected 17 CPAs in tobacco yielded more than 80 %, and reproducibility was found to be better than 20 % of RSD.

참고문헌 (6)

Nobuo Ochiai, Kikuo Sasamoto, Hirooki Kanda and Sadao Nakamura (2006) Fast screening of pesticide multiresidues in aqueous samples by dual stir bar sorptive extraction-thermal desorption-low thermal mass gas chromatography - mass spectrometry. Journal of Chromatography A, 1130:83-90

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Jin'an Cai, Fang Zhu, Wenhong Ruan, Liqin Liu, Rong Lai, Feng Zeng and Gangfeng Ouyang (2013) Determination of organochlorine pesticides in textiles using solid-phase microextraction with gas chromatography -mass spectrometry. Microchemical Journal, 110 : 280-284

상세보기
A. Kende, Z. Csizmazia, T. Rikker, V. Angyal and K. Torkos (2006) Combination of stir bar sorptive extraction - retention time locked gas chromatography - mass spectrometry and automated mass spectral deconvolution for pesticide identification in fruits and vegetables. Microchemical Journal, 84 : 63-69

상세보기
Pat Sandra, Bart Tienpont and Frank David (2003) Multi-residue screening of pesticides in vegetables, fruits and baby food by stir bar sorptive extraction - thermal desorption -capillary gas chromatography - mass spectrometry. Journal of Chromatography A, 1000 : 299-309

상세보기
Erkuden Perez-Carrera, Victor M. Leon Leon, Abelardo Gomez Parra and Eduardo GonzMez-Mazo (2007) Simultaneous determination of pesticides, polycyclic aromatic hydrocarbons and polychlorinated biphenyls in seawater and interstitial marine water samples, using stir bar sorptive extraction - thermal desorption - gas chromatography - mass spectrometry. Journal of Chromatography A, 1070 : 82-90
M. Barriada-Pereira, P. Serodio, M.J. Gonzalez-Castro and J.M.F. Nogueira (2003) Determination of organochlorine pesticides in vegetable matrices by stir bar sorptive extraction with liquid desorption and large volume injection-gas chromatography - mass spectrometry towards compliance with European Union directives. Journal of Chromatography A, 1217 : 119-126

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Development of Fast Screening Method for Crop Protection Agents in Tobacco by Stir Bar Sorptive Extraction and Thermal Desorption coupled to GC/MS 원문보기

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Development of Fast Screening Method for Crop Protection Agents in Tobacco by Stir Bar Sorptive Extraction and Thermal Desorption coupled to GC/MS 원문보기

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