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1428 Pang et al.: Journal of AOAC International Vol. 98, No. 5, 2015
RESIDUES AND TRACE ELEMENTS
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: .
Corresponding author’s e-mail:
DOI: 10.5740/jaoacint.15021
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.
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,
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
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