AOAC 133rd Annual Meeting - Final Program

Poster Abstracts | Tuesday

samples as immunuoaffinity clean-up is particularly effective in removing all pigments from the sample to allow accurate quan- tification by HPLC or LC-MS/MS. IMMUNOPREP ® ONLINE automated affinity cartridges have been developed which offer the same benefits as immunoaffinity column clean-up. Automating analysis offers the added advantage of allowing large scale laboratories to meet increasing pressures with the fastest turn-around times. Sample preparation methods have been validated and tested for the analysis of difficult commodi- ties such as spices and coffee for the automated determination of ochratoxin. Presenter: Elizabeth Manning, R-Biopharm Rhône Ltd, Glasgow, United Kingdom, Email: elizabeth@r-biopharmrhone.com P-T-051 Elaine Marley , Elizabeth Manning , Claire Milligan , Joyce Wilcox , Lynsey Hayes , Gemma Young , R-Biopharm Rhône Ltd, Glasgow, United Kingdom Methods for the Quantitative Measurement of Folic Acid, Biotin, and Vitamin B12 in Health Supplements Vitamins are organic molecules that are necessary for normal metabolism and are either not synthesized in the body or not synthesized in adequate quantities. Consequently, vitamins must be obtained from the diet. There is a growing trend in the number of people taking vitamin supplements which come in a variety of formats. This was also recognised by AOAC as there was an invite in 2016 to submit relevant methods for the quantitative measurement of vitamin B12 in dietary supple- ments and ingredients (AOAC SMPR 2016.017) for review by the AOAC Expert Panel for consideration. As these vita- min supplements were often difficult to analyse, R-Biopharm has developed specific application notes for the analysis of biotin, folic acid and vitamin B12 using immunoaffinity column clean-up. The immunoaffinity columns offer improved clean-up and concentration of the vitamins from the sample giving cleaner chromatograms providing more accurate results and more sensitive detection. The columns contain a specific gel suspension of monoclonal antibody. The vitamin is extracted from the sample and diluted with buffer before applying to the column. Any vitamin which is present in the sample is retained by the antibody within the gel suspension. The column is washed to remove unbound material and the vitamin is then released from the column following elution with solvent prior to analysis by UV-HPLC. A number of different vitamin supplements were analysed during the validation of the method. Presenter: Elizabeth Manning, R-Biopharm Rhône Ltd, Glasgow, United Kingdom, Email: elizabeth@r-biopharmrhone.com P-T-052 Dan Mao , Shanghai Institute for Food and Drug Control, Shanghai, China; Elise Palmer , Nancy Collette , Lingyun Chen , VICAM a Waters Business, Milford, MA, USA Determination of Multi-Mycotoxins in Astragalus Root by Immunoaffinity Purification and LC-MS/MS The expanding use of herbal medicine, and in particular Traditional Chinese Medicine (TCM), leads to an increased

need for effective quality control mechanisms to monitor for mycotoxin contamination during the growth, harvest and storage of cultivated plants. We describe a multi-mycotoxin analytical method, optimized for Astragalus Root, using LC-MS/MS anal- ysis. Sample extraction by orbital shaking with sodium chloride and 70% methanol was followed by clean-up with VICAM’s Myco6in1 + immunoaffinity column. Aflatoxins, ochratoxin A, fumonisins, deoxnivalenol, zearalenone, nivalenol, T-2 and HT-2 toxins were eluted with methanol, dried under nitrogen at 40°C, and reconstituted in acetonitrile/water before injection for anal- ysis. A Waters Acquity UPLC H-class system with CORTECS C 18 column, coupled to a Waters Xevo TQD Mass Spectrometer was used. The linear regression coefficients (r) of all standards were greater than 0.996 over the examined concentration range. The recovery ratio of all mycotoxins was within 73.0-108.2% in matrix, and the precision (RSD%) was less than 8.7%. The LOQs ranged from 0.3-15 µg/kg and were well below the limit required by many countries. This method provides an effective means of monitoring mycotoxins in Astragalus Root. Presenter: Nancy Collette, VICAM a Waters Business, Milford, MA, USA, Email: nancy_zabe_collette@waters.com P-T-053 Joyce Wilcox , Elizabeth Manning , Naomi MacKay , R-Biopharm AG, Glasgow, United Kingdom Analysis of 11 Legislated Mycotoxins in Animal Feed Samples Using a Multi-Analyte Immunoaffinity Column Clean-Up Animal feed matrices present challenges in the extraction, isola- tion and analysis of mycotoxins. Maximum levels permitted in animal feed for each mycotoxin varies according to the type of animal, its age and place in the food chain. Thus, an analytical method must be flexible across a range of required control levels. Detection and quantitation of mycotoxins by LC-MS/MS allows several analytes with diverse physical-chemistry properties to be measured in a single injection whilst providing increased specificity for each analyte. Methods may however be subject to matrix-induced signal suppression or enhancement in the ion source if the sample clean-up is insufficient. Methods based on dilute and shoot extractions, QuEChERS and SPE have been reported, however as sample matrix remains in the final injection solution, this can result in analyte signal suppression and poor sensitivity. Complete matrix removal is desirable and is achieved using immunoaffinity clean-up columns. The 11 + Myco MS-PREP ® column contains antibodies raised to the analytes of interest ensuring excellent recovery of multiple mycotoxins and complete matrix removal. Matrix effects are determined by comparing the response of the mycotoxins spiked onto “blank” sample matrix with the equivalent levels spiked onto solvent “matrix”. Differences of ≤10% indicate the absence of matrix effects and that correction with matrix-matched calibration standards or stable isotope labelled internal standards is unnecessary. Presenter: Elizabeth Manning, R-Biopharm AG, Glasgow, United Kingdom, Email: elizabeth@r-biopharmrhone.com

72 SEPTEMBER 6–12, 2019 SHERATON DENVER DOWNTOWN HOTEL