PMID- 29411087 OWN - NLM STAT- MEDLINE DCOM- 20180911 LR - 20180911 IS - 1618-2650 (Electronic) IS - 1618-2642 (Linking) VI - 410 IP - 22 DP - 2018 Sep TI - Use of a quality control approach to assess measurement uncertainty in the comparison of sample processing techniques in the analysis of pesticide residues in fruits and vegetables. PG - 5465-5479 LID - 10.1007/s00216-018-0905-1 [doi] AB - In routine monitoring of foods, reduction of analyzed test portion size generally leads to higher sample throughput, less labor, and lower costs of monitoring, but to meet analytical needs, the test portions still need to accurately represent the original bulk samples. With the intent to determine minimal fit-for-purpose sample size, analyses were conducted for up to 93 incurred and added pesticide residues in 10 common fruits and vegetables processed using different sample comminution equipment. The commodities studied consisted of apple, banana, broccoli, celery, grape, green bean, peach, potato, orange, and squash. A Blixer(R) was used to chop the bulk samples at room temperature, and test portions of 15, 10, 5, 2, and 1 g were taken for analysis (n = 4 each). Additionally, 40 g subsamples (after freezing) were further comminuted using a cryomill device with liquid nitrogen, and test portions of 5, 2, and 1 g were analyzed (n = 4 each). Both low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS) and ultrahigh-performance liquid chromatography (UHPLC)-MS/MS were used for analysis. An empirical approach was followed to isolate and estimate the measurement uncertainty contribution of each step in the overall method by adding quality control spikes prior to each step. Addition of an internal standard during extraction normalized the sample preparation step to 0% error contribution, and coefficients of variation (CVs) were 6-7% for the analytical steps (LC and GC) and 6-9% for the sample processing techniques. In practice, overall CVs averaged 9-11% among the different analytes, commodities, batches, test portion weights, and analytical and sample processing methods. On average, CVs increased up to 4% and bias 8-12% when using 1-2 g test portions vs. 10-15 g. Graphical abstract Efficient quality control approach to include sample processing. FAU - Lehotay, Steven J AU - Lehotay SJ AD - US Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA, 19038, USA. Steven.Lehotay@ars.usda.gov. FAU - Han, Lijun AU - Han L AD - College of Science, China Agricultural University, Beijing, 100193, China. FAU - Sapozhnikova, Yelena AU - Sapozhnikova Y AD - US Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA, 19038, USA. LA - eng PT - Comparative Study PT - Journal Article DEP - 20180206 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Pesticide Residues) SB - IM MH - Chromatography, High Pressure Liquid/methods MH - Food Contamination/*analysis MH - Food Quality MH - Fruit/*chemistry MH - Gas Chromatography-Mass Spectrometry/methods MH - Hazard Analysis and Critical Control Points/methods MH - Pesticide Residues/*analysis MH - Quality Control MH - Tandem Mass Spectrometry/methods MH - Uncertainty MH - Vegetables/*chemistry OTO - NOTNLM OT - Comminution OT - Fruits and vegetables OT - Measurement uncertainty OT - Pesticide residues analysis OT - Sample processing EDAT- 2018/02/08 06:00 MHDA- 2018/09/12 06:00 CRDT- 2018/02/08 06:00 PHST- 2017/12/08 00:00 [received] PHST- 2018/01/19 00:00 [accepted] PHST- 2018/01/12 00:00 [revised] PHST- 2018/02/08 06:00 [pubmed] PHST- 2018/09/12 06:00 [medline] PHST- 2018/02/08 06:00 [entrez] AID - 10.1007/s00216-018-0905-1 [pii] AID - 10.1007/s00216-018-0905-1 [doi] PST - ppublish SO - Anal Bioanal Chem. 2018 Sep;410(22):5465-5479. doi: 10.1007/s00216-018-0905-1. Epub 2018 Feb 6.