AOAC 133rd Annual Meeting - Final Program

P-M-006 Valerie Toomey , U.S. Food and Drug Administration, Cincinnati, OH, USA Analysis of Performance Enhancing Dietary Supplements for SARMs and Other Doping Compounds Using UHPLC-MS The U.S. Food and Drug Administration (FDA) regulates dietary supplements under the Dietary Supplement Health and Education Act of 1994. The Forensic Chemistry Center regularly receives performance enhancing dietary supplements suspected to contain steroids. An increasing number of these products have been found to contain selective androgen receptor modulators (SARMs). SARMs, such as LGD-4033 and ostarine have similar physiological effects as anabolic steroids, with purportedly less negative side effects. GW501516, a peroxisome proliferator-ac- tivated receptor delta (PPAR δ ) agonist; SR9009 a reversed-viral erythroblastosis (REV-ERB) agonist; and ibutamoren, a nonpep- tide growth hormone secretagogue and a ghrelin receptor agonist have also been identified in these types of products. In October 2017, the FDA warned against using SARMs due to serious safety concerns including potential risks of heart attack, stroke and liver damage. In order to address public health risks, FDA laboratories must provide effective screening methods for these types of compounds in consumer products. A method has been developed to screen dietary supplements for nine SARMs, GW501516, SR9009 and ibutamoren using ultra-high pressure liquid chromatography with mass spectral detection (UHPLC-MS). A gradient using 0.1% formic acid in water and acetonitrile on a C8 column is used to separate the compounds in 9.5 minutes. An ion trap mass spectrometer with electrospray ionization is used for detection. Presenter: Valerie Toomey, U.S. Food and Drug Administration, Cincinnati, OH, USA, Email: valerie.toomey@fda.hhs.gov P-M-007 Congmei Cao , Silva Babajanian , Yanjun Zhang , Peter Chang , Gary Swanson , Herbalife Nutrition, Torrance, CA, USA; Quanyin Gao , Herbalife Manufacturing, Lake Forest, CA, USA NMR Advancements—Food and Dietary Supplement Products Applications NMR is a unique tool for analysis. Compared to the spectro- scopic and chromatographic technologies currently used for analysis in industry, such as HPLC, LC-MS, UV, and IR, NMR is an advanced and efficient technique that provides lot more and repeatable information for analysis with a simple nondestructive sample preparation. It reveals the types and relative amount of atoms present in a sample, the specific environments of atoms within a molecule, the purity and composition of a sample, as well as constitutional and conformational structural information about a molecule. All the information in NMR spectrum could be easily and directly interpreted with help of software and served

L.) is a dietary supplement, currently in use for menopausal issues in women. Milk thistle ( Silybum marianum L.), on the other hand, is beneficial for its anti-inflammatory and anti-viral effects for hepatitis. Due to their importance, there is a need for standardization to ensure consistency in these supplements. UHPLC-MS/MS assays were developed and validated: one for the estrogenic isoflavones and progestin-like flavonoids of red clover and the other assay focused on milk thistle flavo- nolignans. These assays were applied in standardization of botanical dietary supplements from commercial sources and in measurement of the active compounds in serum samples from clinical trials. The linearity range of the proposed method for red clover isoflavones ranged from 0.6–437.4 ng/mL (Genistein), 1.8–437.4 ng/mL (Daidzein and Irilone), 0.3–145.8 ng/mL (Biochanin A), 0.1–145.8 ng/mL (Prunetin), and 0.2–48.6 ng/ mL (Formononetin). The intraday and interday coefficients of vari- ation obtained for the isoflavones were less than 12%. The mean recovery based on low-, medium-, and high-quality control standards ranged between 80 and 108% in serum matrix. The assay method development and validation, application in the standardization of red clover and milk thistle dietary supple- ments, and in the analysis of serum samples from clinical trials will be presented. Presenter: Ruth Muchiri, Oregon State University, Corvallis, OR, USA, Email: muchirir@oregonstate.edu P-M-005 Ken Bolda , NOW Foods, Bloomingdale, IL, USA Alternative Method for the Determination of Chondroitin Sulfate in Dietary Supplements Using a Novel Sample Preparation Approach A novel, simple sample preparation method utilizing hydrochlo- ric acid digestion with pre-column derivatization and HPLC-UV detection was developed and validated for the determination of chondroitin sulfate in dietary supplements. Samples and stan- dards are hydrolyzed in hydrochloric acid and broken down to the amino acid galactosamine. The hydrolysates are derivatized with 6-aminoquinoline- N -hydroxy-succinimidyl carbamate prior to HPLC separation. The target amino acid, galactosamine, is then separated using reverse phase chromatography with UV detection at 260 nm. Galactosamine is quantitated utilizing primary standards to determine the exact amount of chondroi- tin sulfate in samples. The method was carried through a single laboratory validation, which included accuracy, linearity, preci- sion, and determination of limit of quantitation. The technique provides an inexpensive quality control measure for the potency determination of pure chondroitin sulfate powders, mixes containing chondroitin sulfate, and products containing naturally occurring chondroitin sulfate, such as chicken sternal cartilage. Presenter: Ken Bolda, NOW Foods, Bloomingdale, IL, USA, Email: ken.bolda@nowfoods.com

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