Screening for multiple phosphodiesterase type 5 inhibitor drugs in dietary supplement materials by flow injection mass spectrometry and their quantification by liquid chromatography tandem mass spectrometry.
A flow injection tandem mass spectrometry method (FI-MS/MS) has been developed to detect enzyme phosphodiesterase type 5 inhibitors, including tadalafil, sildenafil, and vardenafil. Multiple reaction monitoring (MRM) was used to detect the drugs and product ion ratios were used for identification. FI-MS/MS was used for semi-quantification and liquid chromatography tandem mass spectrometry (LC-MS/MS) was used for further confirmation and quantification. One of 13 samples has been found to be adulterated with prescription levels of tadalafil and also low level of sildenafil. The method can be used for screening large numbers of herbal products for adulteration since it takes less than 1 min without chromatographic separation on a column.
Method Development and Total Diet Research Center, U.S. Food and Drug Administration, 11630 W. 80th Street, Lenexa, KS 66214, USA. fenhong.song@fda.hhs.gov
Fenhong
F
Song
Aref
A
El-Demerdash
Shwn-Ji Susie H
SJ
Lee
D002243:Carbolines / Q000032:analysis; D002853:Chromatography, Liquid; D019587:Dietary Supplements / Q000032:analysis*; D004340:Drug Contamination; D017022:Flow Injection Analysis; D007093:Imidazoles / Q000032:analysis; D013058:Mass Spectrometry / Q000379:methods*; D058986:Phosphodiesterase 5 Inhibitors / Q000032:analysis*; D010879:Piperazines / Q000032:analysis; D028321:Plant Preparations / Q000032:analysis*; D011687:Purines / Q000032:analysis; D000068677:Sildenafil Citrate; D013450:Sulfones / Q000032:analysis; D000068581:Tadalafil; D053719:Tandem Mass Spectrometry; D014227:Triazines / Q000032:analysis; D000069058:Vardenafil Dihydrochloride
D002243:Carbolines; D007093:Imidazoles; D058986:Phosphodiesterase 5 Inhibitors; D010879:Piperazines; D028321:Plant Preparations; D011687:Purines; D013450:Sulfones; D014227:Triazines; D000069058:Vardenafil Dihydrochloride; D000068581:Tadalafil; D000068677:Sildenafil Citrate