AOAC 133rd Annual Meeting - Final Program

Poster Abstracts | Monday

P-M-013 Walter Wilson , Catherine Rimmer , National Institute of Standards and Technology, Gaithersburg, MD, USA Determination of Phenolic Acids in Black Cohosh Standard Reference Materials by Reverse Phase Liquid Chromotography and Photodiode Array Detection Black cohosh ( Cimicifuga racemose L. Nutt.) roots and rhizomes are used worldwide for the treatment of women’s disorders and have been classified as one of the top 10 best-selling herbs in the United States. Adulterated black cohosh supplements have been identified and shown to have hepatotoxicity associated with the supplements prepared with other plant parts then the roots, rhizomes, or different Cimicifuga species. Phenolic acids work as antioxidants to prevent cellular damage due to free-radical oxidation reactions and help promote anti-in- flammatory conditions in the human body. In this study, a new reversed-phase liquid chromatography (RPLC) method coupled to a photodiode array detector (PDA) was developed for the determination of phenolic acids in four candidate black cohosh Standard Reference Materials. A typical two-dimensional chromatogram based on retention time (x-axis) and absorp- tion (y-axis) is extended to a three-dimensional format with the collection of UV spectra (wavelengths, z-axis). The RPLC-PDA method used an ACE 3 C 18 column to determine caffeic acid, ferulic acid, and isoferulic acid in the black cohosh samples. Twelve additional phenolic acid compounds were investigated. Multiple phenolic acids were tentatively identified solely based on retention times. However, the comparison of the UV spectra obtained for reference standards and suspect chromatographic peaks did not match preventing a false identification. Presenter: Walter Wilson, National Institute of Standards and Technology, Gaithersburg, MD, USA, Email: walter.wilson@nist.gov P-M-014 Aboli Girme , Ganesh Saste , Sandeep Pawar , Ruchi Singh , Lal Hingorani , Pharmanza Herbal Pvt Ltd, Anand, India; Bhaumik Darji , Verdure Sciences Inc., Noblesville, IN, USA Withania Somnifera : Recent Investigation and Analysis of Bioactive Markers by LC-PDA-ESI-MS/MS Withania Somnifera (WS) is an increasingly popular botan- ical with current USP methods using only withanoside IV and withanolide A for quantitative analysis of identification mark- ers for WS roots. Extracts of WS roots show the presence of additional markers of withania glycosides and aglycone i.e., withanoside-IV, withanoside-V, withanoside VI, withaferin-A, 27-hydroxywithanolide B (aka 12-Deoxywithastramonolide), withanolide-A, withanone, and withanolide-B. Markers of 27-hydroxywithanone, dihydrowithaferin A and viscosalac- tone B were reported but not quantified in WS root extract. For optimal identification, we have validated a simple LC-MS based method to identify compounds including alkaloids, withanosides, withanolides with withaferin A derivatives in single methodology. In this present study, LC-MS with triple quadrupole was utilized to characterize the compounds present in WS roots, acclaimed for their active biological effects. These are established bioactive markers from withania species and these markers may work as identification and analytical markers of WS. This methodology

will aid in the quality control, authentication, and standardization of this botanical for raw material and extract, critical to dietary supplements. To our knowledge, this is the first complete char- acterization of Withania Somnifera root using a rapid, sensitive, and validated LC-MS method of analysis for identification of bioactive markers. Presenter: Bhaumik Darji, Verdure Sciences Inc., Noblesville, IN, USA, Email: bdarji@vs-corp.com P-M-015 Lizbeth Martinez , Brandon Proctor , Mark Hokenson , Mohamed Koroma , Martin Dennison , Tobe Cohen , Pharmavite, Valencia, CA, USA Single Laboratory Validation of a Method for Determination of Choline in Nutritional Supplements by HPLC with ELS Detection A single laboratory validation study (SLV) was conducted for a High-Performance Liquid Chromatography (HPLC) method with an Evaporative Light Scattering Detector (ELSD) for the deter- mination of Choline in a variety of Prenatal products (tablets, gummies, and softgels) and raw materials. Extraction variants were developed for the different formulation contents. The procedure consisted of extraction with diluent solution and HPLC analysis of the final sample solution using a Waters Xbridge HILIC 5 µ m column. Choline was well separated from other impurities. HPLC test run time per injection is 15 min. On the basis of the accuracy, precision, and recovery results for this study, we highly recommend this quick HPLC method for Choline analysis compared to previous enzymatic methods that are less precise, more time-consuming, and about ten times the cost to execute. Presenter: Lizbeth Martinez, Pharmavite, Valencia, CA, USA, Email: lizmartinez@ucla.edu P-M-016 Daniel Hengst , Andres Vasquez , Tyler Gatz , Chad Scheuerell , Eurofins Food Integrity and Innovation, Madison, WI, USA The Analysis of Retinyl Acetate and Retinyl Palmitate in Foods and Supplements Using Coupled Supercritical Fluid Extraction and Chromatography with Tandem Mass Spectrometry Detection Retinyl Acetate and Retinyl Palmitate are esters of Retinol, also known as Vitamin A. Vitamin A is a critical component of the mammalian dietary intake, having metabolic roles associated with vision, gene transcription and immune function. Due to the nutritional importance of this compound, many foods and supplements are fortified with these ester forms of retinol. The quick and accurate analysis of these compounds is crucial, since dietary deficiency or overabundance may lead to adverse physiological effects. Traditional methodology for the analysis of these compounds can be time consuming and tedious, with lengthy techniques such as saponification and liquid-liquid partitions commonly employed. A method for the analysis of Retinyl Acetate and Retinyl Palmitate has been developed and validated utilizing coupled Supercritical Fluid Extraction and Chromatography with Tandem Mass Spectrometry detection. This technique produces equivalent results to reference methods,

38 SEPTEMBER 6–12, 2019 SHERATON DENVER DOWNTOWN HOTEL