UHPLC-QTOF을 이용한 수산물(바다장어, 넙치, 새우) 중 농약 273성분의 동시분석법 검증
Simultaneous Analysis of 273 Pesticide Multiresidues in Seafood (Conger eel, Flatfish, and Shrimp) Using UHPLC-QTOF
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초록
This study developed and validated a method for the simultaneous analysis of 273 pesticide multiresidues in seafood, specifically targeting conger eel, flatfish, and shrimp, using UHPLC-QTOF. The QuEChERS method was employed for sample preparation, followed by d-SPE purification. Key performance parameters, including method limits of quantitation (MLOQ), linearity, and recovery rates, were evaluated. The results demonstrated that 97.4-98.5% (266-269 analytes) of the pesticides had MLOQs ≤0.01 mg/kg, meeting domestic regulatory standards. Linearity was confirmed with correlation coefficients (r2) greater than 0.980 for 98.5-99.6% (269-272 analytes) of the pesticides, indicating strong relationships between concentration and response. Recovery rates for 92.7-98.9% (253-270 analytes) of the pesticides were within 30-140%, with relative standard deviation (RSD) values ≤20%, demonstrating the method’s analytical suitability in diverse seafood matrices. This validated method provides a robust and efficient tool for monitoring pesticide multiresidues in seafood, contributing to enhanced food safety and public health protection.
Abstract
This study developed and validated a method for the simultaneous analysis of 273 pesticide multiresidues in seafood, specifically targeting conger eel, flatfish, and shrimp, using UHPLC-QTOF. The QuEChERS method was employed for sample preparation, followed by d-SPE purification. Key performance parameters, including method limits of quantitation (MLOQ), linearity, and recovery rates, were evaluated. The results demonstrated that 97.4-98.5% (266-269 analytes) of the pesticides had MLOQs ≤0.01 mg/kg, meeting domestic regulatory standards. Linearity was confirmed with correlation coefficients (r2) greater than 0.980 for 98.5-99.6% (269-272 analytes) of the pesticides, indicating strong relationships between concentration and response. Recovery rates for 92.7-98.9% (253-270 analytes) of the pesticides were within 30-140%, with relative standard deviation (RSD) values ≤20%, demonstrating the method’s analytical suitability in diverse seafood matrices. This validated method provides a robust and efficient tool for monitoring pesticide multiresidues in seafood, contributing to enhanced food safety and public health protection.
참고문헌 (29)
- Hosomi R, "Seafood consumption and components for health", Global Journal of Health Science, 4(3), pp.72~ (2012)[DOI]
- Rani R, "Bacterial Fish Diseases", pp.59~86 (2022), Academic Press
- Damalas CA, "Pesticide exposure, safety issues, and risk assessment indicators", International Journal of Environmental Research and Public Health, 8(5), pp.1402~1419 (2011)[DOI]
- Shin Y, "Liquid chromatography-tandem mass spectrometry for the simultaneous analysis of 353 pesticides in the edible insect Tenebrio molitor Larvae(mealworms)", Molecules, 25(24), pp.5866~ (2020)[DOI]
- Vázquez PP, "Large multiresidue analysis of pesticides in edible vegetable oils by using efficient solid-phase extraction sorbents based on quick, easy, cheap, effective, rugged and safe methodology followed by gas chromatography–tandem mass spectrometry", Journal of Chromatography A, 1463, pp.20~31 (2016)[DOI]
- Dong MW, "Ultra-high-pressure liquid chromatography(UHPLC)in method development", TrAC Trends in Analytical Chemistry, 63, pp.21~30 (2014)[DOI]
- Kruve A, "Tutorial review on validation of liquid chromatography–mass spectrometry methods : Part I", Analytica Chimica Acta, 870, pp.29~44 (2015)[DOI]
- Kruve A, "Tutorial review on validation of liquid chromatography–mass spectrometry methods : Part II", Analytica Chimica Acta, 870, pp.8~28 (2015)[DOI]
- Wang T, "Targeted and non-targeted unexpected food contaminants analysis by LC", HRMS : Feasibility study on rice, 2021, pp.338, 127957~
- Roy-Lachapelle A, "High resolution", accurate mass(HRMS)detection of anatoxin-a in lake water using LDTD–APCI coupled to a Q-Exactive mass spectrometer, 2015, pp.132, 836~844
- Nuñez A, "Characterization of MS", MS product ions for the differentiation of structurally isomeric pesticides by high-resolution mass spectrometry, 2018, pp.6(4), 59~
- Ojanperä S, "Isotopic pattern and accurate mass determination in urine drug screening by liquid chromatography", time-of-flight mass spectrometry, 2006, pp.20(7), 1161~1167
- Kaufmann A, "The current role of high-resolution mass spectrometry in food analysis", Analytical and Bioanalytical Chemistry, 403(5), pp.1233~1249 (2012)[DOI]
- Shin Y, "Liquid chromatography-high resolution mass spectrometry for the determination of three cannabinoids, two(-)-trans-Δ9-tetrahydrocannabinol metabolites, and six amphetamine-type stimulants in human hair", Journal of Chromatography B, 1149, pp.122157~ (2020)[DOI]
- Aguilar-Alarcón P, "Molecular formula assignment of dissolved organic matter by ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry using two non-targeted data processing approaches : A case study from recirculating aquaculture systems", Analytica Chimica Acta, 1288, pp.342128~ (2024)[DOI]
- López A, "Evaluation of sampling adsorbents and validation of a LC-HRMS method for determination of 28 airborne pesticides", Talanta, 189, pp.211~219 (2018)[DOI]
- González-Gaya B, "Suspect and non-target screening : the last frontier in environmental analysis", Analytical Methods, 13(16), pp.1876~1904 (2021)[DOI]
- Jeong MJ, "Simultaneous analysis of 504 pesticide multiresidues in crops using UHPLC-QTOF at MS1 and MS2 levels", Foods, 13(21), pp.3503~ (2024)[DOI]
- Soler C, "Recent trends in liquid chromatography-tandem mass spectrometry to determine pesticides and their metabolites in food", TrAC Trends in Analytical Chemistry, 26(2), pp.103~115 (2007)[DOI]
- Hernández F, "The role of GC-MS", MS with triple quadrupole in pesticide residue analysis in food and the environment, 2013, pp.5(21), 5875~5894
- Sivaperumal P, "Rapid determination of pesticide residues in fruits and vegetables, using ultra-high-performance liquid chromatography", time-of-flight mass spectrometry, 2015, pp.168, 356~365
- Turner JA, "The Pesticide Manual: A World Compendium" (2021), British Crop Production Council
- Harris DC, "Exploring Chemical Analysis" (2013), W. H. Freeman and Company
- Bruice PY, "Essential Organic Chemistry" (2016), Pearson
- Shin Y, "Validation of a multiresidue analysis method for 379 pesticides in human serum using liquid chromatography–tandem mass spectrometry", Journal of Agricultural and Food Chemistry, 66(13), pp.3550~3560 (2018)[DOI]
- Zhang Z, "Multiresidue analysis of pesticides in straw roughage by liquid chromatography–tandem mass spectrometry", Journal of Agricultural and Food Chemistry, 64(31), pp.6091~6099 (2016)[DOI]
- Park E, "Simple and rapid method for 336 multiresidual pesticide analysis in saliva, determination of their chemical stabilities, and biomonitoring of farmers", Chemosphere, 309, pp.136725~ (2022)[DOI]
- Lee J, "Rapid and simultaneous analysis of 360 pesticides in brown rice, spinach, orange, and potato using microbore GC-MS", MS, 2017, pp.65(16), 3387~3395
- Wang X, "Suspect and non-target screening of pesticides and pharmaceuticals transformation products in wastewater using QTOF-MS", Environment International, 137, pp.105599~ (2020)[DOI]