Popularity of natural-based preparations supporting the sexual potency significantly increased in recent years, which also led to the increase of illegal use of phosphodiesterase type 5 inhibitor (PDE-5) in sexual performance enhancement products. In this study, a rapid U-HPLC‒HRMS/MS method has been developed to simultaneously determine 59 PDE-5 inhibitors and their analogues. Within the development of sensitive method for analysis of 59 PDE-5 inhibitors and their analogues, both sample preparation procedure, as well as separation / detection conditions have been optimized. Extraction efficiency of particular extraction solvents, influence of different mobile phase additives on target analytes separation, as well as impact of various settings of mass analyzer on sensitivity of detection were examined. Data were collected in the 'full MS/data dependent MS/MS' acquisition mode (full MS-dd-MS/MS). Before the U-HPLC‒HRMS/MS method was used for analysis of real samples, proper validation had been conducted. The precision of the method expressed as the relative standard deviation (RSD) was ≤4.2% and ≤5.2% at spiking concentrations 5 μg/g and 0.25 μg/g, respectively. The limits of quantification were in the range 0.25 - 0.05 μg/g and the recovery ranged between 71 and 90%. The optimized method was successfully applied for analysis of 64 real samples, and 10 of them were proved to contain both registered or unregistered synthetic PDE-5 inhibitors. Additionally, the acquired U-HPLC‒HRMS/MS fingerprints were demonstrated to serve as an efficient tool for revealing of other type of possible fraud in products labeling. Retrospective mining of markers of herbs declared on dietary supplements packaging allowed to assess the trueness / untruth in the declaration of medical herbs composition.
- MeSH
- fytonutrienty analýza normy MeSH
- inhibitory fosfodiesterasy 5 analýza MeSH
- kontaminace léku prevence a kontrola MeSH
- limita detekce MeSH
- padělané léky analýza MeSH
- podvod prevence a kontrola MeSH
- potravní doplňky analýza normy MeSH
- tandemová hmotnostní spektrometrie metody MeSH
- vysokoúčinná kapalinová chromatografie metody MeSH
- Publikační typ
- časopisecké články MeSH
- Geografické názvy
- Česká republika MeSH
Counterfeit steroids are available on the black market, ultimately to consumers who believe they are buying a legitimate pharmaceutical item from the labeled company. In many cases, counterfeit steroids can contain lower doses or some products can be overdosed. This can unwittingly expose users to a significant health risks. The mixture of testosterone propionate, phenylpropionate, isocaproate and decanoate in an oil-based injectable dosage form belongs to the one of the most misused illicit drugs by a variety of athletes. This study developed a new, fast, simple and reliable HPLC method combined with a simple sample preparation step to determine testosterone propionate, phenylpropionate, isocaproate and decanoate in an oil-based injectable dosage form without the use of sophisticated and expensive instrumentation. The developed analytical procedure provides high throughput of samples where LC analysis takes only 6min and sample preparation of oil matrix in one step takes approximately 10min with precision ranging from 1.03 to 3.38% (RSD), and accuracy (relative error %) within ±2.01%. This method was found to be precise, linear, accurate, sensitive, selective and robust for routine application in screening of commercial pharmaceutical products based on content of mentioned testosterone esters in their oil-based injectable dosage form for counterfeit drugs. This method was successfully applied to the analysis of nine samples of commercial testosterone mixtures purchased from various sources and will be further used as an effective screening method for determination of previously mentioned testosterone esters in samples confiscated by Institute of Forensic Science (Slovakia) during the illegal trade.
False drugs are unsafe products that are manufactured using incorrect, inactive, or harmful ingredients. These drugs are packaged and labeled to look like real trademark generic drugs to deceive the consumer. Chemical analysis is a crucial step in distinguishing original pharmaceutics and fakes. HPLC and MS analyses are standard methods for identification and quantitation of active ingredients and impurities. Thus they are often used to corroborate the results of less sophisticated methods such as colorimetry, TLC, GS, Raman, NIR, FTIR and NMR spectrometries. The analytical methods should be employed in forensic laboratories.
- MeSH
- artemisininy * analýza klasifikace MeSH
- chemické techniky analytické * metody využití MeSH
- chromatografie na tenké vrstvě metody využití MeSH
- chromatografie plynová metody využití MeSH
- farmaceutický průmysl zákonodárství a právo MeSH
- hmotnostní spektrometrie metody trendy využití MeSH
- inhibitory fosfodiesteras * analýza MeSH
- kolorimetrie metody využití MeSH
- kontaminace léku * prevence a kontrola zákonodárství a právo MeSH
- lidé MeSH
- magnetická rezonanční spektroskopie metody MeSH
- padělané léky * analýza zásobování a distribuce MeSH
- Ramanova spektroskopie metody MeSH
- spektroskopie infračervená s Fourierovou transformací metody přístrojové vybavení využití MeSH
- vysokoúčinná kapalinová chromatografie metody využití MeSH
- Check Tag
- lidé MeSH
