Abstract:
: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.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Jiru M,Stranska-Zachariasova M,Dzuman Z,Hurkova K,Tomaniova M,Stepan R,Cuhra P,Hajslova Jdoi
10.1016/j.jpba.2018.11.007subject
Has Abstractpub_date
2019-02-05 00:00:00pages
713-724eissn
0731-7085issn
1873-264Xpii
S0731-7085(18)31185-3journal_volume
164pub_type
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journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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abstract::An analytical method to study the bioavailability of newly developed pentoxifylline sustained-release tablets has been developed and assessed in experiments on dogs. For the isolation of pentoxifylline and its metabolites from serum solid-liquid extraction was applied by involving the internal standard probe. HPTLC pl...
journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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abstract::Phytochemical investigation of the methanolic extract of Byrsonima crassifolia's bark led to the isolation of 8 known phenolic compounds 5-O-galloylquinic acid, 3-O-galloylquinic acid, 3,4-di-O-galloylquinic acid, 3,5-di-O-galloylquinic acid, 3,4,5-tri-O-galloylquinic acid, (+)-epicatechin-3-gallate along with (+)-cat...
journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,评审
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journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
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abstract::A new herbal health product marketed for enhancing erectile function, namely Power58 Platinum, was purchased over-the-counter in Hong Kong. The product was tested for adulteration with sildenafil, tadalafil, and vardenafil as well as their structurally modified analogues. A new analogue of vardenafil, in which the N-e...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2007.12.004
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journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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doi:10.1016/j.jpba.2012.08.025
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journal_title:Journal of pharmaceutical and biomedical analysis
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abstract::Functional cell-based assays are the preferred method to test for the presence of anti-rHuEPO neutralizing antibodies (NAbs). However, due to the unpredictable nature of test serum matrix effects on cell-based assays, confirmatory assays are essential for verifying NAb positive results observed during the course of sa...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2011.03.029
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abstract::A methylene blue (MB) poly(vinyl chloride) membrane sensor based on MB-silicotungstate (SLT) ion association as electroactive material was described. The linear response covered the range 1 x 10(-3)-1 x 10(-6) mol x dm(-3) MB solution, with a slope 52.0+/-0.8 mV decade(-1) (pH range 3.0-10.0). The detection limit was ...
journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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abstract::A highly sensitive and selective liquid chromatography-tandem mass spectrometry method for the determination of tetrahydrocannabinol (THC), cannabidiol, and rimonabant in rat plasma was developed. Analytes and the internal standard were extracted from plasma using a combination of protein precipitation followed by liq...
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abstract::Delivery of small interfering RNAs (siRNAs) into cells still remains a challenge in gene delivery studies. Here, we investigated the ability of synthesized Fe3O4-PEG-LAC-chitosan-PEI nanoparticles for siRNA delivery of survivin as the model gene into cells. The cellular uptake of survivin siRNA carried by synthesized ...
journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
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abstract::Direct spray such as leaf spray and paper spray ionization mass spectrometry (MS) is a powerful type of ambient MS for phytochemical analysis. In this paper, direct spray MS methods to rapidly distinguish and analyze five species of Callicarpa L. have been developed. To distinguish species, leaf spray MS was employed ...
journal_title:Journal of pharmaceutical and biomedical analysis
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journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,meta分析,评审
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abstract::Metabolism of the tricyclic azaphenothiazine neuroleptic drug prothipendyl was investigated with in vitro studies using human liver microsomes but also specific isoforms of cytochrome P450 (CYP) enzymes. Identification and analysis of metabolites was done by liquid chromatography (LC) coupled with quadrupole time of f...
journal_title:Journal of pharmaceutical and biomedical analysis
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