Separation of 1,3‐dimethylamylamine and other polar compounds in a dietary supplement formulation using aqueous normal phase chromatography with MS

Abstract

Five ingredients (caffeine, L-arginine, creatine, β-alanine, and 1,3-dimethylamylamine) from a workout supplement were separated by HPLC with UV detection and LC-MS using an analytical column based on silica hydride operating in aqueous normal phase mode. While RP methods were observed to be inadequate for the analysis due to low retention, aqueous normal phase chromatography was able to readily retain and resolve the analytes. After method development on the HPLC-UV system, the conditions were successfully transferred to an LC-MS system for analysis. Based on calibration curve data, estimates of 63.5, 380.3, and 13.1 mg/serving (5.50 g) were obtained for creatine, l-arginine, and 1,3-dimethylamylamine, respectively. Standard addition data results were compared to those of the calibration curve study, and the two values differed by less than 1% in the case of creatine. The conditions are suitable for further development as a reliable means of quantitating the analytes in workout supplement formulations.

Phenolic composition of pomegranate peel extracts using an liquid chromatography-mass spectrometry approach with silica hydride columns

“…A perfluorinated phase demonstrated significant retention capabilities in both the RP and aqueous normal phase modes . The dual retention capabilities of various silica hydride phases have been used effectively for the determination of such diverse analytes as drugs of abuse , dietary supplements , and hydrophobic and hydrophilic bases .…”

Pharmacokinetic and Toxicological Aspects of 1,3-Dimethylamylamine with Clinical and Forensic Relevance

“…Detection of the presence of 1,3-DMAA in supplements can be achieved through different methods, such as high-performance liquid chromatography with a UV detector (HPLC-UV) and liquid chromatography with mass spectrometry (LC-MS) [80], direct analysis in real-time tandem mass spectrometry (DART-MS/MS) [20], a combination of direct analysis in real time with a high-resolution quadrupole time-of-flight mass spectrometer (DART-QToF-MS) [33], 63 Ni ionization ion mobility spectrometry (IMS) and electrospray ionization-high-performance ion mobility spectrometry-mass spectrometry (ESI-HPIMS-MS) [81], 1 H nuclear magnetic resonance (NMR) spectroscopy [82,83], ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) [29], derivatization with trifluoroacetic anhydride (TFAA) followed by gas chromatographyhigh-resolution time-of-flight mass spectrometry (GC-high-resolution-TOFMS) with soft ionization [84], among others. These techniques have been applied for different matrices, such as blood [3,7], dried blood spots [85], whole blood sample (postmortem) [43], urine [8,86] and exhaled breath [87].…”

Synthesis and Characterization of Molecularly Imprinted Polymer with Dimethylamylamine as Template

“…Based on the assumption, each side of adsorption has the same affinity for the template molecule. Adsorption on one side does not affect the other side [8]. Based on the value of ∆G in Table-2, the isotherm adsorption model follows the Langmuir isotherm model with the energy generated at MIP of -19.167 (J/mol) and at NIP of -15.405 (J/mol).…”

“…These developed methods require complex procedures and expensive analysis instruments resulting from heterogeneous sample matrices. It is necessary to develop a separation method with high selectivity to analyte [8].…”