AOAC 133rd Annual Meeting - Final Program

Poster Abstracts | Wednesday

P-W-008 Fang Chou , Chia-Ling Chang , Ching-Yi Huang , Taipei City Government, Taipei, Taiwan; Yu-Hsuan Lin , Yu-Han Huang , Yi-Jun Lin , Guor-Jien Wei , National Yang Ming University, Taipei, Taiwan Analysis of Safrole in Soft Drinks Safrole was mainly derived from the sassafras plant and 80% of essential oil extracted from sassafras plant is safrole. Safrole was considered to be carcinogenic to animals but lacked evidence for human carcinogenicity (Group 2B) by International Agency for Research on Cancer (IARC). Safrole can’t be used in food, however, it might present as a residue of plant extracts added in soft drink with the maximum residue limit for 1 ppm in the United States. Saforle was a legal flavor additive in soft drinks in Taiwan and the maximum residue limit was 1.0 ppm. According to the source of safrole, it might contain impurities such as isosafrole and myristicin. Impurities could be used to determine whether the source of safrole was plant extraction or chemical synthe- sis. This study refers to Method of Test for Safrole in Soft Drinks designed to determine the safrole levels in different soft drinks sampled by the Taiwan official GC/MS/MS method and LOQ of safrole was 10 ppb. In addition, we developed methods to extract and quantify myristicin to determine whether the source of safrole was plant extraction or chemical synthesis. This study analyzed safrole in 15 soft drink samples, 11 of 15 samples were non-detected. Other 4 samples, the concentration of safrole were 12.05-16.17 ppb and the concentration of myristicin were 56.91-113.04 ppb. Moreover, the source of safrole in these 4 soft drinks is plant extraction. Presenter: Fang Chou, Taipei City Government, Taipei, Taiwan, Email: fangchou@health.gov.tw P-W-009 J.D. De-Alwis , Euan Ross , Joanne Williams , Eimear McCall , Waters Corp., Wilmslow, United Kingdom Acrylamide is a well-known carcinogenic contaminant formed at high temperatures during the cooking of starch containing foods. Acrylamide hit the headlines again internationally in 2018, when a judge in California ruled acrylamide fell under the State’s Proposition 65 labeling requirements and EU Regulation 2017/2158 was enacted establishing mitigation measures and benchmark levels for the reduction of the presence of acrylamide in food in Europe. The analysis of acrylamide in processed foods has several analytical challenges to consider, including sufficient retention, the complexity of the matrices and the wide range concentrations likely. A new method, using modified QuEChERS and LC-MS/MS with a high strength silica C18 analytical column, has been developed, to provide a rapid, cost-effective approach for quantifying acrylamide in coffee. Solid phase extraction (SPE) and dispersive solid phase extraction (dSPE) devices were evaluated, to identify simple and efficient cleanup of the samples, to provide selective MRM transitions. Single laboratory method validation was completed using a selection of store purchased coffee products and a coffee reference material. Determination of Acrylamide in Coffee by Liquid Chromatography-Tandem Quadrupole Mass Spectrometry

Acrylamide-d3 was used as an internal standard to correct for any variability through the whole method, including any LC-MS/ MS matrix effects. Validation of the method demonstrated excel- lent performance in terms of linearity, accuracy, precision, and repeatability. Presenter: Eimear McCall, Waters Corp., Wilmslow, United Kingdom, Email: eimear_mccall@waters.com P-W-010 Stuart Adams , J.D. De-Alwis , Joanne Williams , Euan Ross , Eimear McCall , Waters Corp., Wilmslow, United Kingdom Determination of Pesticides in Edible Oils Detection of pesticides in olive oil has many challenges due to the complexity of the matrix which is high in lipids. Sample cleanup is, therefore, crucial to ensure robust methodology. Traditional methods involved liquid-liquid extraction followed by gel permeation chromatography (GPC) cleanup. This technique is undesirable due to high solvent consumption and lengthy extraction and cleanup times. This poster presents an alternative, extraction and cleanup procedure optimized for the simple and reliable determination of multi-residue pesticides in edible oils by GC-MS/MS. Edible oils were homogenized and spiked with known concentrations of pesticides. The extraction was opti- mized, followed by a simple pass through cleanup. All extracts were run on GC-EI-MS/MS, in MRM mode, using a splitless injection of 1 µL. Validation was completed in accordance with European guidelines (SANTE/11813/2017) evaluating sensitiv- ity, selectivity, repeatability, accuracy and identification criteria. Excellent linearity, over the calibration range of 0.005 to 0.1 mg/kg, was achieved for all pesticides with coefficients of deter- mination > 0.995 with residuals <20%. The method’s accuracy, repeatability and bias was evaluated from the analysis of spikes at 0.01 mg/kg (n=5), 0.02 mg/kg (n=5) and 0.1 mg/kg (n=5). Presenter: Eimear McCall, Waters Corp., Wilmslow, United Kingdom, Email: eimear_mccall@waters.com P-W-011 Xiuqin Li , Hongmei Li , National Institute of Metrology, Beijing, China Development and Validation of LC-IDMS Method on Measurement of Veterinary Drug Residues in Food In the present study, we developed a comprehensive strategy to determine accurately veterinary residues in food by LC-IDMS, which can increase the selectivity, sensitivity and throughput toward the identification and quantification of compounds in samples. It is well known that the presence of co-extracted matrix can severely affect the quantification procedures based on ESI and APCI LC-MS methods, which is called matrix effects. As a matter of fact, ME is becoming a major threat to the successful application of LC-ESI-MS. Several operational strategies have been suggested to minimize the interference of co-eluting matrix compounds. They include extensive cleanup procedures prior to LC-MS/MS analysis and more efficient chromatographic separations and the use of isotope-labeled internal standards. A systematic, comprehensive strategy which optimizes sample

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