Nutritional Outlook

Nutritional Outlook, April 2018

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■ NUTRITIONAL OUTLOOK 16 Supplement Safety APRIL 2018 Oxilofrine has been studied in animals and humans and found to cause ef ects on the heart similar to those cause by ephedrine. Ac- cording to our research, 26 adverse events have been reported in the Netherlands linked to sup- plements containing oxilofrine. T ese supple- ments led to nausea and vomiting, tachycardia, chest pain, and cardiac arrest. Additionally, ox- ilofrine is often disguised on labels as "methyl- synephrine" or "extract of Acacia rigidula." Another example is DMAA. In 2013, I worked with researchers at the U.S. Army Research In- stitute of Environmental Medicine (USARIEM) and determined that DMAA is not "natural" in origin and should not be used as an ingredi- ent in dietary supplements. T e f ndings sup- port research conducted by academic research laboratories around the world. Several sports supplements have tried to market DMAA as a natural constituent of geranium or its extract, but there is no credible scientif c evidence to support that claim. Products containing DMAA have been linked to health problems and at least f ve deaths. T e FDA issued several warning letters to manufacturers who have formulated their products with DMAA and urged consumers to avoid these products. Sev- eral professional and Olympic athletes have lost their eligibility to compete due to the presence of DMAA in their system. Stores and online re- tailers, however, still sell products that contain DMAA, despite the FDA ban. How We Test for Adulterants When testing products for banned substances, I usually "target" what adulterant I am search- ing for, purchase a reference standard for that adulterant, and then test for the adulterant. In targeted analysis, I use ultra-high-performance liquid chromatography (UHPLC) coupled with tandem mass spectrometry to detect and mea- sure compounds. In the case of the Clini- cal Toxicology study, however, I had to deviate from that process after f nding that the adulterant we originally targeted—2-aminoisoheptane— was not in all of the products. At this point, we shifted to an "untargeted" or investigative approach. T e Clinical Toxicology investigative analysis was really interesting in that I used a dif erent technique to capture much of the in- formation and then "sifted out" the interesting features. I still used UHPLC, but coupled that with a high-resolution/accurate mass spec- trometer (HRAM-MS). T is instrumentation is capable of measuring a compound's mass with a high degree of accuracy and dif erentiate it from others close in mass. For instance: tes- tosterone has a molecular formula of C 19 H 28 O 2 , which corresponds to an exact mass of 288.2089. Desoxymethyltestosterone has a mo- lecular formula of C 20 H 32 O and a corresponding exact mass of 288.2453. A typical quadrupole mass spectrometer would not be able to dis- tinguish between the two. T e HRAM-MS is selective enough to be able to distin- guish between those two and provide an accurate mass mea- surement to the third decimal place for each. I analyzed all of the products in the Clinical Toxicology study using the UHPLC-HRAM-MS instrument and examined their interesting features. First, I identif ed the features that corresponded to the labeled ingredients. T en I worked on identifying the remaining fea- tures, working on those with the most intense to the least intense signals. It was in this way that I uncovered the presence of the unlabeled ingredients. I still had to use the targeted method—UHPLC coupled with tandem mass spectrometry—with a reference standard to conf rm the presence and quantity of ingredi- ents. T is last step, using a reference standard to characterize ingredients during testing, is very important; unfortunately, some research- ers omit this step in published research. An Opportunity to Set Yourself Apart While the vast majority of manufacturers are committed to quality and safety, a small num- ber of manufacturers continue to develop and market products that contain potentially harmful ingredients. Some might say this pres- ents a great opportunity for reputable com- panies that want to showcase their products' quality and safety to set themselves apart. T ird-party certif cation of dietary and sports supplements, such as my organization's NSF International certif cation program, helps companies dif erentiate their products. When consumers see the NSF certif cation mark on a package, they can be sure those vitamins and supplements have been independently tested for harmful levels of specif c contaminants like lead and arsenic and that label claims have been verif ed. My colleagues and I are already working on several new research projects in- volving hidden stimulants in supplements. We expect to publish our f ndings this year. Reference 1. Cohen PA et al., "Four experimental stimulants found in sports and weight loss supplements: 2-amino-6-methylheptane (octodrine), 1,4-di- methylamylamine (1,4-DMAA), 1,3-dimeth- ylamylamine (1,3-DMAA) and 1,3-dimethyl- butylamine (1,3-DMBA)," Clinical Toxicology. Published online November 8, 2017. John Travis has more than 20 years of expe- rience as an analytical chemist specializing in the analysis of dietary supplements. As senior research scientist, dietary supple- ments, at global public health organization NSF International (Ann Arbor, MI), Travis analyzes hundreds of dietary supplement products each year for various contami- nants, emerging drugs, and harmful com- pounds. He is a subject matter expert on athletic banned substances and was instru- mental in the development of the screening methods used for the NSF International Cer- tif ed for Sport program, which now screens products for more than 270 banned sub- stances on the World Anti-Doping Agency, National Football League, Major League Baseball, and National Collegiate Athletic Association lists. Travis is currently involved with the analysis of pharmaceutical agents and illicit drugs, stimulants, and other pro- hibited substances as both adulterants and contaminants in dietary supplements and functional foods, co-authoring scientif c papers on ingredients of concern includ- ing stimulants drugs DMAA, DEPEA, and DMBA found in dietary supplements. HO H N H N OH OH CH 3 CH 3 CH 3 CH 3 Oxilofrine (-) - Ephedrine NH 2 NH 2 Amphetamine 1,3-Dimethylamylamine

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