1428 Pang et al. : J ournal of AOAC I nternational V ol. 98, N o. 5, 2015


High Throughput Analytical Techniques for the Determination and Confirmation of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea by GC/MS, GC/MS/MS, and LC/MS/MS: Collaborative Study, First Action 2014.09 Guo-Fang Pang and Chun-Lin Fan Chinese Academy of Inspection and Quarantine, No. 3 Gaobeidian North Rd 100123, Chaoyang District, Beijing, People’s Republic of China Yan-Zhong Cao Qinhuangdao Entry-Exit Inspection and Quarantine Bureau, No. 1 Liupanshan Rd 066004, Qinhuangdao, Hebei, People’s Republic of China Fang Yan Fujian Entry-Exit Inspection and Quarantine Bureau, No. 312 Hudong Rd, Fuzhou, Fujian, People’s Republic of China Yan Li, Jian Kang, Hui Chen, and Qiao-Ying Chang Chinese Academy of Inspection and Quarantine, No. 3 Gaobeidian North Rd 100123, Chaoyang District, Beijing, People’s Republic of China Collaborators: R. Boni; A. Chakraborty; Z.-M. Chen; A.R. Fernandez; Q.-L. Guo; G.-T. Han; V. Hanot; D.-L. Huang; S.-M. Huang; Y.-J. Huang; N. Kanamaru; U. Karasek; J. Kuballa; A. Kwasniok; M. Lambert; I. Lederer; Y.-R. Lee; M. Lehneke; H.-P. Li; L. Liu; F.-J. Luo; C. Lüllmann; A. Lozano; V. Merlo; T. Rawn; J. Reuther; W.-B. Song; C.-H. Tu; X.-Y. Wang; Z.-Y. Wang; L.-Q. Xie; K. Yu; R. Zhang

Received January 22, 2015. The method was approved by the Expert Review Panel for Pesticide Residues as First Action. The Expert Review Panel for Pesticide Residues invites method users to provide feedback on the First Action methods. Feedback from method users will help verify that the methods are fit for purpose and are critical to gaining global recognition and acceptance of the methods. Comments can be sent directly to the corresponding author or Supplemental Tables 18–23, Figures 4 and 5, and Annexes 1–3 are available on the J. AOAC Int. website: http://aoac.publisher. Corresponding author’s e-mail: DOI: 10.5740/jaoacint.15021 Since there were no restrictions regarding the type of analytical instrumentation to use for the analyses, laboratories used a combination of equipment that included GC/MS, GC/MS/MS, and LC/MS/MS instruments from 22 different manufacturers, 21 brands of GC and LC columns, 13 different GC temperature programming profiles, Thirty laboratories from fom North and South America, Europe, and Asia participated in this AOAC collaborative study (15 from China; five from Germany; two each from Italy and the United States; and one each from the Republic of Korea, Canada, Spain, Japan, Belgium, and India). Participants represented government regulatory, commercial testing, university, research institute, and private laboratories. The single-laboratory validated (SLV) tea method was evaluated in the collaborative study to determine the recovery and reproducibility of the method under multilaboratory conditions.

11 LC gradient elution programs, and six different vendor manufactured SPE cartridges. Even though all the analytical performance parameters for all the 653 compounds had been determined in the SLV study, guidance was obtained from an expert review panel of the AOAC Method-Centric Committee on Pesticide Residues to conduct the multilaboratory collaborative study based on 20 selected compounds that can be analyzed by GC/MS and 20 compounds that can be analyzed by LC/MS/MS. Altogether, 560 samples covering the 40 selected pesticides were analyzed in the study. These samples included green tea and oolong tea samples fortified typically at the European Union maximum residue limit for regulatory guidance and compliance, aged tea samples incurred with 20 pesticides, and green tea and oolong tea samples incurred with five pesticides. The analysis of the 560 samples generated a total of 82459 test results by the 30 participating laboratories. One laboratory failed to meet the proficiency requirements in the precollaborative study. Therefore, its data submitted for the collaborative study were excluded from further analysis and interpretation. The results presented are therefore the 6638 analytical results obtained from the 29 remaining laboratories, which included 1977 results generated by GC/MS, 1704 results by GC/MS/MS, and 2957 results by LC/MS/MS. It was determined after application of the Grubbs and Dixon tests for outliers to the data sets that there were 65 outlier results from the 1977 GC/MS results (3.3%), 65 outlier results from the

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