Gas Chromatographic Determination of Pesticide Residues Using Electron-capture Detector and Mass Spectrometry

다국어 초록 (Multilingual Abstract)

The sensitive and reliable method for determination of 6 pesticides, cyanazine (triazine), uniconazole (azole),diflufenican (nicotinilide), vernolate (thiocarbamate),bromoxynil (hydroxyl benzonitrile), and asulam (sulfanilyl carbamate) were examined and validated. The methods based on solid-phase extraction (SPE) and gas chromatograph (GC) with electron capture detection (ECD). Confirmation analysis of pesticides was carried out by GC-MS in the selected ion monitoring (SIM) mode using 2 target ions.
Method validation was performed at 5 fortification levels (0.005, 0.01, 0.05, 0.1, and 0.5 mg/L). The linearity of the calibration curves was excellent in matrix matched standards,and yielded the coefficients of determination (R2)≥0.9982for all target analytes. The limit of quantification (LOQ)was 0.05 mg/L for 6 pesticide compounds and the reporting level of the method, defined as lower than the maximum residue levels established by Korea Food &Drug Administration (KFDA). Average recoveries of the pesticides spiked at 0.05, 0.1, and 0.5 mg/L into 3agricultural products, rice, apple, and soybean were in the range 76.40-120% with relative standard deviation (RSD)values ≤11.07% for all compounds, respectively.

참고문헌 (Reference)

1 Pang GF, "Validation study on 660 pesticide residues in animal tissues by gel permeation chromatography cleanup/gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry" 1125 : 1-30, 2006

2 Hirahara Y, "Validation of multiresidue screening methods for the determination of 186 pesticides in 11 agricultural products using gas chromatography" 51 : 617-627, 2005

3 Lehotay SJ, "Validation of a fast and easy method for the determination of 229 pesticide residues in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection" 88 : 595-614, 2005

4 Bolles HG, "U.S. market basket study to determine residues of the insecticide chlorpyrifos" 47 : 1817-1822, 1999

5 Yune YP, "The manual of pesticide residue analysis" Korea Food & Drug Administration 2009

6 Hennion MC, "Solid-phase extraction: Method development, sorbents, and coupling with liquid chromatography" 856 : 3-54, 1999

7 Fytianos K, "Solid phase microextraction applied to the analysis of organophosphorus insecticides in fruits" 65 : 2090-2095, 2006

8 de la Colina C, "Simultaneous determination of various pesticides in water by solid-phase extraction/HPLC with photodiode array detection" 153 : 1-6, 1994

9 Ascherio A, "Schwarzschild MA, Thun MJ. Pesticide exposure and risk for parkinson's disease" 60 : 197-203, 2006

10 Lee YD, "Practical handbook of pesticide residue analysis in food code" National Institute of Food and Drug Safety Evaluation 2009

11 Sherma J, "Pesticide residue analysis: A review" 84 : 1303-1312, 1999

12 Colosio C, "Neurobehavioral effects of pesticides: State of the art" 24 : 577-591, 2003

13 Yang X, "Multiresidue method for determination of 88 pesticides in berry fruits using solid-phase extraction and gas chromatography-mass spectrometry: Determination of 88 pesticides in berries using SPE and GC-MS" 127 : 855-865, 2011

14 Hernandez F, "Multiresidue liquid chromatography tandem mass spectrometry determination of 52 non-gas chromatography-amenable pesticides and metabolites in different food commodities" 1109 : 242-252, 2006

15 Ueno E, "Multiresidue analysis of pesticides in agricultural products by GCECD after GPC and graphitized carbon column cleanup" 45 : 212-217, 2004

16 Queiroz SCN, "Methods of extraction and/ or concentration of compounds found in biological fluids for subsequent chromatographic determination" 24 : 68-76, 2001

17 Vinas P, "Method development and validation for strobilurin fungicides in baby foods by solid-phase microextraction gas chromatographymass spectrometry" 1216 : 140-146, 2009

18 Lambropoulou DA, "Headspace solid-phase microextraction in combination with gas chromatography-mass spectrometry for the rapid screening of organophosphorus insecticide residues in strawberries and cherries" 993 : 197-203, 2003

19 Fernandez-Alvarez M, "Development of a solid-phase microextraction gas chromatography with microelectron-capture detection method for a multiresidue analysis of pesticides in bovine milk" 617 : 37-50, 2008

20 Ganzera M, "Development and validation of an HPLC/UV/MS method for simultaneous determination of 18 preservatives in grapefruit seed extract" 54 : 3768-3772, 2006

21 Kim DH, "Determination of organophosphorus pesticides in wheat flour by supercritical fluid extraction and gas chromatography with nitrogen-phosphorus detection" 824 : 63-70, 1998

22 Costa LLF, "Determination of herbicides used in irrigated rice cultivation in the south of Santa Catarina using SPME-GC-ECD" 31 : 83-, 2008

23 Moorman PG, "Consumption of dairy products and the risk of breast cancer: A review of the literature" 80 : 5-14, 2004

24 Acquavella J, "Cancer among farmers: A meta-analysis" 8 : 64-74, 1998

25 Choi JS, "Can auto-id make trade stable between Korea and China" 7 : 119-127, 2004

26 Blasco C, "Analysis of pesticides in fruits by pressurized liquid extraction and liquid chromatography-ion traptriple stage mass spectrometry" 1098 : 37-43, 2005

27 Henriksen T, "Analysis of metribuzin and transformation products in soil by pressurized liquid extraction and liquid chromatographic.tandem mass spectrometry" 957 : 79-87, 2002

28 Zheng T, "Agricultural exposure to carbamate pesticides and risk of nonhodgkin lymphoma" 43 : 641-649, 2001