AOAC 133rd Annual Meeting - Final Program

Poster Abstracts | Wednesday

CA, USA; Roland Carlson , California Department of Food And Agriculture, Sacramento, CA, USA nDATA: What it is and Why Multi-Residue Labs Should Care? This poster presents the development and validation of a univer- sal screening approach, based on accurate mass measurement, that can be tailored to any multi-residue pesticide lab’s needs. Based on hybrid high-resolution mass spectrometer platforms, this approach implements an expandable, flexible and search- able compound database using proprietary processing software. This combination allows for screening of multi-residue samples without the need for a complete standard suite and semi-auto- mated data processing. Coined as non-Target Data Acquisition for Data Analysis or nDATA, this approach can be used for risked based screening or program based monitoring. The nDATA approach was validated using a UHPLC/ESI Q-Orbtrap mass spectrometer (Q-Exactive). Extraction was done by QuEChERs and a single sample injection took only 14 minutes. Five fruits (apple, banana, grape, orange, and strawberry) and five vegetables (broccoli, carrot, lettuce, potato and tomato) were used for method validation with SANTE/11813/2017 screening criteria as a reference. Metrics used for nDATA screening criteria included retention time and accurate mass measurements of the precursor and fragments. These metrics were acquired for each compound and compiled into compound databases (CDB) for semi-automated data processing. The vali- dated nDATA approach was able to screen for 845 pesticides (and 105 veterinary drugs). Presenter: Jian Wang, Canadian Food Inspection Agency (CFIA), Calgary, AB, Canada, Email: jian.wang2@canada.ca P-W-046 Huan Lin , Toshiya Matsubara , Natsuyo Asano , Shimadzu Japan, Kyoto, Japan; Mikie Shima , AiSTI Science, Wakayama, Japan; Alan Owens , Shimadzu USA, Columbia, MD, USA Targeted Screening and Quantitation of Pesticide Residues in Green Tea Using a Quadrupole Time-of-Flight Mass Spectrometer With population growth and the development of agriculture and food industries, food safety is becoming a greater concern in recent years. The increasingly stricter regulations of residual food contaminants requires faster and more accurate analytic techniques. For this purpose, targeted screening by simultaneous MRM measurements using a triple quadrupole mass spec- trometer is the most common strategy. Data acquisition using a high-resolution and accurate mass spectrometer (HRMS), such as a Time-of-Flight, is also carried out coupled with MRM-based analysis for the purpose of guaranteeing the robustness and reliability of screening. In addition, HRMS also provides a differ- ent advantage from MRM measurement because a compound which was not included as a target when acquiring data can be processed later without reacquiring data. The purpose of this study is to screen and identify pesticide chemicals in green tea. Compounds from green tea were extracted with QuEChERS method and analyzed with MS/MS measurement using a LC/Q-TOF-MS.

Presenter: Alan Owens, Shimadzu USA, Columbia, MD, USA, Email: amowens@shimadzu.com P-W-047 Nozomi Maeshima , Manami Kobayashi , Junichi Masuda , Shimadzu Japan, Kanagawa, Japan; Alan Owens , Shimadzu USA, Columbia, MD, USA Simultaneous Determination of Pesticide Residues in Vegetable Extract by Liquid Chromatograph Tandem Mass Spectrometry for High Recovery Rate In order to protect the food safety, it is important to establish detection criteria of pesticide residues and methods to improve the accuracy for measuring the concentration of the targets. In Japan, the detection criteria of pesticide residues are established as the Positive List System by the Ministry of Health, Labor and Welfare, as well as the standard test methods. For monitoring of pesticide by LC-MS/MS, recovery rate should be the criti- cal issue in addition to sensitivity. Generally, standard addition method as well as matrix-matched calibration curve are useful techniques rather than absolute calibration method in order to reduce matrix effects; however, these techniques are not always appropriate methods since each sample requires its independent calibration curve, respectively, for a wide variety of samples. In this report, we introduce the results of investigation for basic parameters around the ESI ionization to avoid matrix effects and to maximize recovery rate of target pesticides using abso- lute calibration methods. This poster describes the development of simultaneous determination of pesticide residues in food by LC-MS/MS. Presenter: Alan Owens, Shimadzu USA, Columbia, MD, USA, Email: amowens@shimadzu.com P-W-048 Tara Nickel , Christine Casey , Wendy Andersen , U.S. Food and Drug Administration, Denver, CO, USA Determination of Pentobarbital in Pet Foods and Ingredients of Animal Origin Used in Pet Food by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) Pentobarbital is a barbiturate drug commonly used in animals as a sedative, anesthetic, or for euthanasia. FDA considers pet foods with any detectable level of pentobarbital adulterated and are in violation of the Federal Food, Drug, and Cosmetic Act. Beginning in 2017, pentobarbital contamination has triggered the recall of several canned pet foods. The source of the contam- ination has been linked to tallow supplied to the dog food manufacturers. For ongoing analysis of pentobarbital in tallow and dog food products, it was highly desirable to use a quick extraction procedure with application to a variety of different product types, yielding accurate quantitative and confirmatory results suitable for routine regulatory analysis. The determina- tion of pentobarbital in meat (horse, beef, pork, lamb, goat and venison), rendering streams (tallow, meat and bone meal, meat byproducts meal) and finished dog and cat food products was done with a simple shakeout extraction with acetonitrile, dilu- tion, and analysis via LC-MS/MS. Pentobarbital was separated using an Agilent Eclipse Plus-C18 LC column and detected using negative mode electrospray ionization (ESI) on a SCIEX QTRAP 5500 hybrid linear ion trap mass spectrometer. Samples

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