Dietary Supplements — How Safe are they?

Maybe you take a multi-vitamin pill every morning, or perhaps use a whey protein supplement to increase performance at the gym. But did you know that these consumer products are not subject to the same scrutiny as pharmaceutical drug formulations? A manufacturer does not need to demonstrate efficacy before sale to the general public. Indeed, it is only after the product has been demonstrated to be “adulterated or misbranded” by the FDA can action be taken to halt production, distribution, and sale. Recently, this has in fact happened with some dietary supplements containing compounds like aegeline or 1,3-dimethylamylamine (DMAA). These compounds are not APIs in any currently used pharmaceutical formulation and scientific study of their safety for human consumption is nebulous at best. On the contrary, they have been implicated in deleterious health issues up to and including death when taken in dietary supplement products.
                We investigated protein sport mix dietary supplements in our laboratory and were able to separate and detect both aegeline and DMAA in these samples. Use of LC-MS allowed for further specificity with EICs of the analytes. We used both reversed phase and ANP methods with the Cogent Bidentate C18 2.o™ and Diamond Hydride™ columns depending on the analytes. I think these method approaches will become more valuable in the years to come; as the FDA begins to crack down more heavily on dietary supplement manufacturers with tighter regulation, there will be an exigent need for reliable analytical methods.
                Not only did we discover aegeline or DMAA in the samples, we also found other ingredients not listed on the label. Here we observed creatine and caffeine present in one formulation. Although these compounds may not be as dangerous as aegeline or DMAA, this finding may be important for some people who need to reduce or eliminate their intake of creatine or caffeine yet are unaware of their presence in the product. The bottom line is that consumers should have a clear understanding of what the product contains and how it may impact their health to make an informed purchasing decision.  
                Click here to read the full study.

Say goodbye to complex sample prep!

Today’s laboratory is becoming increasingly automated and streamlined. Indeed, one of the most time-consuming tasks in your lab is likely to be sample prep which often requires several manual steps. Ideally, we would all like to use a simple “dilute-and-shoot” approach for every analysis but because of interferences from the sample matrix, this is not always possible. 

                I investigated three simple strategies which you can use to avoid sample cleanup steps like SPE. The first uses the Cogent Diamond Hydride™ column to retain the analyte by a different mechanism. When I tried to analyze folic acid in cereal by reversed phase, I found interfering peaks co-eluting with the analyte peak. In aqueous normal phase (ANP) with the Diamond Hydride™, most of the matrix peaks eluted at the solvent front while folic acid was retained.

                The next approach can be used where matrix contaminants build up on the column. You can elute these in a wash step incorporated into the injection sequence. How often you need to do the wash will depend on the complexity of the samples but I found every six injections for orange juice samples was enough.

                The third approach uses LCMS. More sophisticated detection methods can provide you with additional specificity. When analyzing histamine in red wine, I found vast differences between the complex total ion chromatogram (TIC) and the clean extracted ion chromatogram (EIC). Hence, peaks that can co-elute with histamine may be resolved using MS specificity.

                You may be able to avoid sample cleanup steps using one or all of these strategies. Read more in our Extended Application Note.