Screening for multiple weight loss and related drugs in dietary supplement materials by flow injection tandem mass spectrometry and their confirmation by liquid chromatography tandem mass spectrometry

Song, Fenhong; Monroe, Douglas; El-Demerdash, Aref; Palmer, Cynthia A.

doi:10.1016/j.jpba.2013.08.031

Cited by 41 publications

(20 citation statements)

References 17 publications

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“…Adulteration is an exemplary repercussion of such laxity. Well documented are instances of diuretics, stimulants, anorectics, or oxidative uncouplers contained in weight loss supplements [60][61][62][63][64][65][66][67][68][69][70][71][72][73][74], steroids in performance enhancers [75][76][77][78][79][80], and phosphodiesterase 5 inhibitors contained within male enhancement products [72,74,[81][82][83][84][85][86][87][88][89][90][91][92][93]. At least nine people died in Sweden following exposure to Kratom adulterated with Odesmethyltramadol, a potent opioid analgesic.…”

Section: Supplement Regulationmentioning

confidence: 99%

Suspected Adulteration of Commercial Kratom Products with 7-Hydroxymitragynine

et al. 2016

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Introduction Kratom (Mitragyna speciosa), a plant native to Southeast Asia, has been used for centuries for its stimulant and opium-like effects. Mitragynine and 7-hydroxymitragynine, exclusive to M. speciosa, are the alkaloids primary responsible for Kratom's biologic and psychoactive profile, and likely contribute to its problematic use. We purchased several commercially available Kratom analogs for analysis and through our results, present evidence of probable adulteration with the highly potent and addictive plant alkaloid, 7-hydroxymitragynine. Methods A simple and sensitive LC-MS/MS method was developed for simultaneous quantification of mitragynine and 7-hydroxymitragynine in methanol extract of marketed Kratom supplements. Results We found multiple commercial Kratom products to have concentrations of 7-hydroxymitragynine that are substantially higher than those found in raw M. speciosa leaves. Conclusions We have found multiple packaged commercial Kratom products likely to contain artificially elevated concentrations of 7-hydroxymitragynine, the alkaloid responsible for M. speciosa's concerning mechanistic and side effect profile. This study describes a unique form of product adulteration, which stresses the importance of increased dietary supplement oversight of Kratom-containing supplements.

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Section: Supplement Regulationmentioning

confidence: 99%

Suspected Adulteration of Commercial Kratom Products with 7-Hydroxymitragynine

et al. 2016

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“…(FIA)–MS/MS has been widely utilized as a simple and high‐throughput method in comparison with LC‐hyphenated techniques. It provides cost‐ and time‐effective strategies that have been explored for the analysis of pharmaceuticals in different matrices . For example, a fully validated simple FIA‐MS/MS method was recently developed to quantify metformin in dog serum .…”

Section: Introductionmentioning

confidence: 99%

Rapid and simple flow injection analysis tandem mass spectrometric method for the quantification of melphalan in a lipid‐based drug delivery system

Mohammed-Saeid

Michel

Badea

et al. 2017

Rapid Comm Mass Spectrometry

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Rationale: The use of the anticancer drug melphalan is limited due to its poor water solubility.To address this limitation, it is incorporated within a novel delivery system using β-cyclodextringemini surfactants (18:1βCDg).Methods: Herein, two fast and simple flow injection analysis/tandem mass spectrometric (FIA-MS/MS) methods are developed for the quantification of melphalan (Mel) within the drug delivery system so that the solubilization efficiency of the system can be assessed. FIA-MS/MS methods are developed using a triple quadrupole linear ion trap mass spectrometer, equipped with electrospray ionization (ESI) in the positive ion mode. A deuterated form of melphalan (melphalan-d8) was used as an internal standard (IS). The methods were validated according to the FDA guidance.Results: A linearity in the range of 2-100 ng/mL and accuracy and precision below 15% were observed for all standard points and quality control samples. The intra-and inter-day variations and freeze-thaw stability were within the acceptable range according to the criteria set by regulatory guidelines. On the other hand, other stability measures, such as room temperature stability and long-term stability, did not meet the required guidelines in some cases, indicating the need for quick sample analysis upon preparation. Such a fact could have been overlooked if full method validation had not been performed. Conclusions:The developed methods were applied to determine the encapsulation/ solubilization of the [18:1βCDg/Mel] delivery system. 18:1βCDg enhances the aqueous solubility of melphalan without the need for co-solvent. The highest melphalan solubility was observed at a melphalan18:1βCDg/Mel complex molar ratio of 2:1. This study demonstrated that a fast analysis for the purpose of quantifying a chemically unstable drug, such as melphalan, is feasible and important for the development of commercial dosage forms.

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“…This method has been tested on multiple PDE-5is in dietary supplements including sildenafil, tadalafil, and vardenafil [65]. Another study was carried out for weight-loss drugs including sibutramine and its analogues [66]. Tests were positive on comparing the ratios of referenced standards with the MRM calculations of the adulterants.…”

Section: Mass Spectrometry-based Techniquesmentioning

confidence: 99%

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2016

Planta Med

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Screening for multiple weight loss and related drugs in dietary supplement materials by flow injection tandem mass spectrometry and their confirmation by liquid chromatography tandem mass spectrometry

Cited by 41 publications

References 17 publications

Suspected Adulteration of Commercial Kratom Products with 7-Hydroxymitragynine

Suspected Adulteration of Commercial Kratom Products with 7-Hydroxymitragynine

Rapid and simple flow injection analysis tandem mass spectrometric method for the quantification of melphalan in a lipid‐based drug delivery system

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