Method Validation for the Analysis of Multiple Weight Loss Drugs in Dietary Supplement Materials by LC-MS/MS
DOI:
https://doi.org/10.21423/JRS-V03N02P015Keywords:
weight loss drugs, sibutramine, LC-MS/MSAbstract
A method validation is reported for the detection and quantification of multiple weight loss drugs in dietary supplement materials. The sample preparation was followed as described in LIB 4549 and the mass spectral measurements were accomplished using liquid chromatography tandem mass spectrometry with electrospray ionization. A method validation was performed at various fortification levels (250 and 1000 g/g) for all 11 drug compounds. The overall recoveries with standard deviation averaged 93.8 6.65% with the majority of individual recoveries in the range of 76% - 110%. The overall limits of quantification (LOQ) for analytes averaged at 10 ng/g. An overall indicator of linearity (R2) averaged at 0.9993 (0.0 250.0 ng/mL). The precision of five replicates of the 50 ng/mL level averaged at 98.4 0.41% with < 1%.
https://doi.org/10.21423/jrs-v03n02p015 (DOI assigned 8/7/2019)
References
P. R. F. Song, D. Monroe, A. Demerdash, C. Palmer, Screening for multiple weight loss drugs in dietary supplement materials by flow injection tandem mass spectrometry and their confirmation by liquid chromatography tandem mass spectrometry, Laboratory Information Bulletin 4549.
F. M. S. R. Gratz, C. L. Flurer, K. A. Wolnik, Analysis of undeclared synthetic phosphodiesterase-5 inhibitors in dietary supplements and herbal matrices by lc-esi-ms and lc-uv, J. Pharm. Biomed. Anal. 36.
I. . S. E. Edison, S. R. Gratz, B. M. Gamble, A. S. Mohrhaus, Lc-ms/ms method for sibutramine and related compounds, Laboratory Information Bulletin 4477.
Tainted products marketed as dietary supplements potentially dangerous. www.fda.gov/NewsEvents/Newsroom/PressAnnouncements/2010/ucm236967.htm Web accessed December 2015.
Dietary Supplement Analysis Quality Assurance Program. http://www.nist.gov/mml/csd/organic/dsqap.cfm. Web accessed December 2015.
Guidance for Industry Mass Spectrometry for Confirmation of the Identity of Animal Drug Residues. http://www.fda.gov/downloads/AnimalVeterinary/ GuidanceComplianceEnforcement/GuidanceforIndustry/ucm052658.pdf. Web accessed December 2015.
Slim-30 Herb Supplement: Undeclared Drug Ingredient. http://www.fda.gov/Safety/MedWatch/ SafetyInformation/SafetyAlertsforHumanMedicalProducts/ucm219463.htm. Web accessed December 2015.
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