title: Rapid and Simultaneous Analysis of 360 Pesticides in Brown Rice, Spinach, Orange, and Potato Using Microbore GC-MS/MS.
abstract: A multiresidue method for the simultaneous and rapid analysis of 360 pesticides in representative agricultural produce (brown rice, orange, spinach, and potato) was developed using a modified QuEChERS procedure combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). Selected reaction monitoring transition parameters (e.g., collision energy, precursor and product ions) in MS/MS were optimized to achieve the best selectivity and sensitivity for a wide range of GC-amenable pesticides. A short (20 m) microbore (0.18 mm i.d.) column resulted in better signal-to-noise ratio with reduced analysis time than a conventional narrowbore column (30 m × 0.25 mm i.d.). The priming injection dramatically increased peak areas by masking effect on a new GC liner. The limit of quantitation was <0.01 mg/kg, and the correlation coefficients (r2) of matrix-matched standards were >0.99 within the range of 0.0025-0.1 mg/kg. Acetonitrile with 0.1% formic acid without additional buffer salts was used for pesticide extraction, whereas only primary-secondary amine (PSA) was used for dispersive solid phase extraction (dSPE) cleanup, to achieve good recoveries for most of the target analytes. The recoveries ranged from 70 to 120% with relative standard deviations of ≤20% at 0.01 and 0.05 mg/kg spiking levels (n = 6) in all samples, indicating acceptable accuracy and precision of the method. Seventeen real samples from local markets were analyzed by using the optimized method, and 14 pesticides in 11 incurred samples were found at below the maximum residue limits.
authors.affiliation: Department of Agricultural Biotechnology, Seoul National University , Seoul 08826, Republic of Korea.
authors.forename: Jonghwa
authors.initials: J
authors.lastname: Lee
authors.affiliation: School of Applied Biosciences, Kyungpook National University , Daegu 41566, Republic of Korea.
authors.forename: Leesun
authors.initials: L
authors.lastname: Kim
authors.affiliation: Department of Agricultural Biotechnology, Seoul National University , Seoul 08826, Republic of Korea.
authors.forename: Yongho
authors.initials: Y
authors.lastname: Shin
authors.affiliation: Department of Agricultural Biotechnology, Seoul National University , Seoul 08826, Republic of Korea.
authors.forename: Junghak
authors.initials: J
authors.lastname: Lee
authors.affiliation: Department of Agricultural Biotechnology, Seoul National University , Seoul 08826, Republic of Korea.
authors.forename: Jiho
authors.initials: J
authors.lastname: Lee
authors.affiliation: Department of Agricultural Biotechnology, Seoul National University , Seoul 08826, Republic of Korea.
authors.forename: Eunhye
authors.initials: E
authors.lastname: Kim
authors.affiliation: Department of Plant Life and Environmental Sciences, Hankyong National University , Anseong 17579, Republic of Korea.
authors.forename: Joon-Kwan
authors.identifier: http://orcid.org/0000-0001-9944-7475
authors.initials: JK
authors.lastname: Moon
authors.affiliation: Department of Agricultural Biotechnology, Seoul National University , Seoul 08826, Republic of Korea.
authors.forename: Jeong-Han
authors.identifier: http://orcid.org/0000-0001-5094-7954
authors.initials: JH
authors.lastname: Kim
mesh_terms: D032084:Citrus sinensis / Q000737:chemistry*; D005506:Food Contamination / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D012275:Oryza / Q000737:chemistry*; D010573:Pesticide Residues / Q000737:chemistry*; D011198:Solanum tuberosum / Q000737:chemistry*; D018724:Spinacia oleracea / Q000737:chemistry*
chemical_list: D010573:Pesticide Residues
keywords: GC-MS/MS; QuEChERS; brown rice; orange; pesticide multiresidues; potato; spinach