Characterization of a new illicit phosphodiesterase-type-5 inhibitor identified in the softgel shell of a dietary supplement.

Abstract:

:A new sildenafil analog has been identified in the softgel shell of a dietary supplement. The compound was investigated by UV spectroscopy and high-resolution MS analysis, leading to the proposed structure 1-methyl-5-{5-[2-(4-methylpiperazin-1-yl)acetyl]-2-propoxyphenyl}-3-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one. A synthetic reference compound with the proposed structure was prepared, and the two sets of analytical data were compared, confirming the structure of the new compound. The compound was named propoxyphenyl noracetildenafil from its structure and similarity with the known compound.

journal_name

J Pharm Biomed Anal

authors

Doi T,Takahashi K,Yamazaki M,Asada A,Takeda A,Kiyota K,Tagami T,Sawabe Y,Yamano T

doi

10.1016/j.jpba.2018.08.031

subject

Has Abstract

pub_date

2018-11-30 00:00:00

pages

61-65

eissn

0731-7085

issn

1873-264X

pii

S0731-7085(18)31276-7

journal_volume

161

pub_type

杂志文章
  • LC-MS/MS method for simultaneous determination of viramidine and ribavirin levels in monkey red blood cells.

    abstract::A high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed for the simultaneous determinations of total viramidine (viramidine, viramidine monophosphate, viramidine diphosphate, and viramidine triphosphate) and total ribavirin (ribavirin, ribavirin monophosphate, ribavirin d...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2006.09.001

    authors: Yeh LT,Nguyen M,Dadgostari S,Bu W,Lin CC

    更新日期:2007-02-19 00:00:00

  • Development and validation of a HPLC method for routine quantification of the decapeptide Cetrorelix in liposome dispersions.

    abstract::The development and validation of an HPLC method for the quantification of the decapeptide Cetrorelix (acetyl-D-2-naphthylalanyl-D-4-chlorphenylalanyl-D-3-pyridylalanyl-seryl-tyrosyl-D-citrullyl-leucyl-arginyl-prolyl-d-alaninamide), a potent antagonist of the luteinising hormone-releasing hormone in liposome dispersio...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2003.11.010

    authors: Grohganz H,Schläfli O,Rischer M,Brandl M

    更新日期:2004-03-10 00:00:00

  • Simultaneous automated image analysis and Raman spectroscopy of powders at an individual particle level.

    abstract::Solid form diversity of raw materials can be critical for the performance of the final drug product. In this study, Raman spectroscopy, image analysis and combined Raman and image analysis were utilized to characterize the solid form composition of a particulate raw material. Raman spectroscopy provides chemical infor...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2020.113744

    authors: Sekulovic A,Verrijk R,Rades T,Grabarek A,Jiskoot W,Hawe A,Rantanen J

    更新日期:2021-01-30 00:00:00

  • A sensitive HPLC-UV method for quantifying vancomycin in biological matrices: Application to pharmacokinetic and biodistribution studies in rat plasma, skin and lymph nodes.

    abstract::Vancomycin (VCN) is an antibiotic used in the treatment of methicillin-resistant Staphylococcus aureus (MRSA)-derived infections. As it has a relatively narrow therapeutic window, it is imperative to develop a sensitive and reliable analytical method for drug monitoring and pharmacokinetic purposes. In the present stu...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2020.113429

    authors: Ramadon D,Courtenay AJ,Permana AD,Tekko IA,McAlister E,McCrudden MTC,McCarthy HO,Donnelly RF

    更新日期:2020-09-10 00:00:00

  • Method optimization of hydrophilic interaction chromatography separation of nucleotides using design of experiment approaches I: Comparison of several zwitterionic columns.

    abstract::A systematic method in hydrophilic interaction chromatography (HILIC) was developed for the separation of four monophosphate nucleotides using design of experiment (DOE) approaches. Three HPLC parameters, the buffer concentration (ammonium acetate concentration), gradient time, and temperature, were evaluated within t...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2018.05.014

    authors: Arase S,Kimura S,Ikegami T

    更新日期:2018-09-05 00:00:00

  • Fast and single solid phase fluorescence spectroscopic batch procedure for (acetyl) salicylic acid determination in drug formulations.

    abstract::A solid phase fluorescence spectroscopic batch procedure for (acetyl) salicylic acid in drug formulations have been developed. The procedure is based on the sorption of salicylic acid (SA) on Sephadex DEAE A-25 anion exchanger gel (100 mg) by equilibration from an aqueous solution (10 or 25 ml) for 5 min; the equilibr...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(02)00719-7

    authors: Ortega Algar S,Ramos Martos N,Molina Díaz A

    更新日期:2003-03-10 00:00:00

  • Development of a liquid chromatographic method for the simultaneous quantification of curcumin, β-arteether, tetrahydrocurcumin and dihydroartemisinin. Application to lipid-based formulations.

    abstract::A liquid chromatographic method was developed for the simultaneous separation of curcumin, β-arteether, tetrahydrocurcumin and dihydroartemisinin based on the design of experiments and the design space methodology. The influence of the percentage of organic modifier, flow rate of the mobile phase and column temperatur...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2013.09.009

    authors: Memvanga PB,Mbinze JK,Rozet E,Hubert P,Préat V,Marini RD

    更新日期:2014-01-01 00:00:00

  • Determination of bopindolol in pharmaceuticals by capillary isotachophoresis.

    abstract::Capillary isotachophoresis (ITP) with conductimetric detection has been used for separating and determining bopindolol (I) in commercial mass-produced pharmaceutical preparations. The optimised operational electrolyte system consisted of 5 mM potassium picolinate and 5 mM picolinic acid (leading electrolyte, LE; pH 5....

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(01)00671-9

    authors: Urbánek M,Pospísilová M,Polásek M

    更新日期:2002-05-15 00:00:00

  • Capillary electrophoresis for caffeine and pyroglutamate determination in coffees study of the in vivo effect on learning and locomotor activity in mice.

    abstract::In a preliminary study pyroglutamate showed to be over 10 times increased in some lyophilised coffees with respect to brewed or filtered coffees, and probably that increase is related to some stage of the industrial process. Pyroglutamate is known to have a number of remarkable cognitive enhancing effects, which could...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2006.01.062

    authors: Maeso N,del Castillo C,Cornejo L,García-Acicollar M,Alguacil LF,Barbas C

    更新日期:2006-06-16 00:00:00

  • Bioactive phenols in algae: the application of pressurized-liquid and solid-phase extraction techniques.

    abstract::A new extraction technique based on the off-line combination of pressurized-liquid with solid-phase extraction (PLE-SPE) is described. The method was used for the extraction of bioactive phenolic acids (protocatechuic, p-hydroxybenzoic, 2,3-dihydroxybenzoic, chlorogenic, vanillic, caffeic, p-coumaric, salicylic acid),...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2009.03.027

    authors: Onofrejová L,Vasícková J,Klejdus B,Stratil P,Misurcová L,Krácmar S,Kopecký J,Vacek J

    更新日期:2010-01-20 00:00:00

  • Effective separation and analysis of E- and Z-guggulsterones in Commiphora mukul resin, guggulipid and their pharmaceutical product by high performance thin-layer chromatography-densitometric method.

    abstract::A high performance thin-layer chromatographic (HPTLC) method for the simultaneous determination of the hypolipidemic agents, E- and Z-isomers of guggulsterone in Commiphora mukul resin, guggulipid (ethyl acetate extract of resin), and its pharmaceutical formulation, was developed. The developed system was efficient en...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2011.05.021

    authors: Musharraf SG,Iqbal N,Gulzar U,Ali A,Choudhary MI,Atta-Ur-Rahman

    更新日期:2011-09-10 00:00:00

  • Determination of LAG078, a lipid-lowering compound, in dog plasma using liquid chromatography-tandem mass spectrometry: application in a toxicokinetic study.

    abstract::A high throughput method was developed and validated for the quantitative determination of LAG078, a lipid-lowering compound, in dog plasma obtained during toxicokinetic studies. The method was based on reverse phase liquid chromatographic separation of the analyte from plasma extract followed by turbo-ionspray (TIS) ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2004.02.020

    authors: Majumdar TK,Wu S,Vedananda S,Tse FL

    更新日期:2004-06-29 00:00:00

  • Determination of tyrosine kinase inhibitor afatinib in rat plasma using LC-MS/MS and its application to in vivo pharmacokinetic studies of afatinib liposomes.

    abstract::A sensitive quantitative liquid chromatography-tandem mass spectrometry assay for afatinib in rat plasma was developed and validated using afatinib dimaleate as a standard. The analyte was determined to be ionized using the positive ion multiple reaction monitoring mode through electrospraying on an AB Sciex Triple Qu...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2018.10.043

    authors: Lu X,Liu S,Yang X,Han M,Sun K

    更新日期:2019-02-05 00:00:00

  • Liquid chromatographic determination of amoxycillin and clavulanic acid in pharmaceutical preparations.

    abstract::A liquid chromatographic method for the simultaneous determination of amoxycillin and potassium clavulanate in tablet and suspension preparations is presented. The method specifies reversed phase column and a buffered mobile phase (CH3OH + KH2PO4-buffer pH 6 + H2O, 15:1:84) isocratically at a rate of 1.0 ml min-1, wit...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(91)80214-t

    authors: Abounassif MA,Abdel-Moety EM,Mohamed ME,Gad-Kariem RA

    更新日期:1991-01-01 00:00:00

  • 19F and 1H magnetic resonance strategies for metabolic studies on fluorinated xenobiotics: application to flurbiprofen [2-(2-fluoro-4-biphenylyl)propionic acid].

    abstract::Strategies for the use of 1H and 19F nuclear magnetic resonance (NMR) spectroscopy as an aid to the study of the metabolic fate of fluorinated drugs are discussed with reference to the application of these methods to flurbiprofen metabolism in man. 1H and 19F NMR analysis of untreated urine enabled the detection of tw...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(90)80067-y

    authors: Wade KE,Wilson ID,Troke JA,Nicholson JK

    更新日期:1990-01-01 00:00:00

  • Seventeen O-acetylated N-glycans and six O-acetylation sites of Myozyme identified using liquid chromatography-tandem mass spectrometry.

    abstract::O-acetylated sialic acid (SA) attached to the N-glycans of therapeutic glycoproteins reportedly inhibit sialidase activity, increase protein half-life, decrease protein antigenicity, and stabilize protein conformation. Recombinant human acid α-glucosidase (Myozyme) is the only drug approved by the United States Food a...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2019.03.013

    authors: Park H,You S,Kim J,Kim W,Do J,Jang Y,Kim D,Lee J,Ha J,Oh DB,Kim JI,Kim HH

    更新日期:2019-05-30 00:00:00

  • Relationship between retention characteristics and physicochemical parameters of solutes on porous graphitized carbon column.

    abstract::The retention of 44 barbituric acid derivatives was determined on porous graphitized carbon (PGC) column using dioxane water mixtures as eluents. Linear correlations were calculated between the logarithm of the capacity factor and the dioxane concentration in the eluent. Free Wilson analysis combined with stepwise reg...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(98)00205-2

    authors: Forgács E,Cserháti T

    更新日期:1998-12-01 00:00:00

  • Concurrent quantification and comparative pharmacokinetic analysis of bioactive compounds in the Herba Ephedrae-Semen Armeniacae Amarum herb pair.

    abstract::The Mahuang-Xingren herb-pair (MX), the combination of Herba Ephedrae (Mahuang in Chinese) and Semen Armeniacae Amarum (Xingren in Chinese), is a classical combination used in traditional Chinese Medicine to treat asthma and bronchitis. A simple and reliable ultra-performance liquid chromatography-tandem mass spectrom...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2015.02.004

    authors: Song S,Chen F,Xing X,Ren M,Ma Q,Xie Y,Tang Q,Luo J

    更新日期:2015-05-10 00:00:00

  • Determination and pharmacokinetics of DT-13 in rat plasma by LC-MS.

    abstract::A sensitive and specific LC-MS assay for DT-13 in rat plasma was developed. DT-13 is an active steroidal saponin present in Liriopes Radix and is developed as an anti-tumor drug candidate. The samples were extracted by acetonitrile-mediated plasma protein precipitation. The chromatographic separation was carried out u...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2011.07.003

    authors: Chen LL,Yuan WW,Hu ZF,Qi J,Zhu DN,Yu BY

    更新日期:2011-11-01 00:00:00

  • A simple method to monitor serum concentrations of fluoxetine and its major metabolite for pharmacokinetic studies.

    abstract::A rapid, selective and sensitive isocratic reversed-phase HPLC assay coupled with MS/MS detection for simultaneous quantification of fluoxetine and its major active metabolite in serum samples has been developed. Analytes were extracted with a simple three step liquid-liquid procedure and chromatographic separation wa...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2008.11.017

    authors: Franceschi L,Faggiani A,Furlanut M

    更新日期:2009-02-20 00:00:00

  • Development and validation of a fully automated LC method for the determination of cloxacillin in human plasma using anion exchange restricted access material for sample clean-up.

    abstract::In the framework of a preliminary investigation on the plasma profile of cloxacillin after oral administration, a simple and rapid LC method was developed for the direct determination of this compound in human plasma. The on-line sample clean-up was carried out using a weak anion exchanger (diethylaminoethyl groups) a...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2004.09.017

    authors: Rbeida O,Chiap P,Lubda D,Boos KS,Crommen J,Hubert P

    更新日期:2005-01-04 00:00:00

  • Fine structural characterization of sulodexide.

    abstract::Sulodexide is a heparinoid which combines the properties of its components heparin and dermatan sulfate and is used not only for the prophylaxis and treatment of thromboembolic diseases but also for the treatment of diabetic nephropathy. Despite many clinical studies have been conducted to investigate its activity and...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2018.04.012

    authors: Veraldi N,Guerrini M,Urso E,Risi G,Bertini S,Bensi D,Bisio A

    更新日期:2018-07-15 00:00:00

  • Pharmacokinetics and tissue distribution of a bioactive sesquiterpenoid from Polygonum jucundum following oral and intravenous administrations to rats.

    abstract::Polygonum jucundum is a traditional Chinese medicine used for the treatment of diseases. The major bioactive compound in the ethanol extract of P. jucundum is 2α-hydroxyl-3β-angeloylcinnamolide (HAC), a drimane-type sesquiterpenoid, which possesses anti-inflammatory activities. The purpose of this study was to investi...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2013.04.033

    authors: Zhang F,Gong X,Xiao B,Zhang C,Wang Z

    更新日期:2013-09-01 00:00:00

  • Comparison of liquid chromatography and capillary electrophoresis methods for quantification of sodium residuals.

    abstract::Liquid chromatography (LC) and capillary electrophoresis (CE) methods were developed to perform the determination of residual sodium in mother liquors and successive washes of an active pharmaceutical ingredient (API). The addition of sodium chloride to the product solution results in rapid and complete crystallizatio...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2006.07.020

    authors: Briône W,Herbots C,Köttgen C,Loix S,Gibella M,Bertrand M,Ceccato A

    更新日期:2007-07-27 00:00:00

  • Development of a laboratory robotic system for automated bioanalytical methods--II. A robot computer program for guarding totally automated bioanalytical methods.

    abstract::The application of fully automated, unattended sample preparation performed by a laboratory robot for the analysis of drugs in biological samples requires the prevention of system failures which may arise in the on-line coupled chromatographic system or in other components of the robotic system. A computer program has...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(90)80083-2

    authors: Wieling J,Hempenius J,Jeuring HJ,Jonkman JH,Coenegracht PM,Doornbos DA

    更新日期:1990-01-01 00:00:00

  • Forced degradation studies of medroxyprogesterone acetate injectable suspensions (150 mg/ml) with implementation of HPLC, mass spectrometry, and QSAR techniques.

    abstract::Medroxyprogesterone acetate (MPA) injectable products are a key commodity for reproductive health and are available in the global market from a variety of manufacturing sources. Depending on the climatic zone conditions of the destination country for product use, MPA injectables are at risk of exposure to adverse tran...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2020.113352

    authors: Jenkins D,Harmon CL,Jia X,Kesselring A,Hatcher D,Grayson K,Ayres J

    更新日期:2020-08-05 00:00:00

  • Assay and purity analysis of diatrizoate sodium in drug product by LC.

    abstract::An LC procedure was developed to separate diatrizoate sodium from three known impurities. These impurities are 2,4- and 2,6-diiodo-3,5-diacetamidobenzoic acid (DDZA), and the free amine (5-acetamido-3-amino-2,4,6-triiodobenzoic acid). The separation was achieved using a Hamilton, PRP-X100, anion exchange column. The r...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(97)00007-1

    authors: Chellquist EM,Nelson WO,Storflor HL

    更新日期:1997-09-01 00:00:00

  • Rapid analysis of benzodiazepines in whole blood by high-performance liquid chromatography: use of a monolithic column.

    abstract::In a previous work [J. Pharm. Biomed. Anal. 23 (2000) 447] a rapid high-performance liquid chromatography (HPLC) method, using a monolithic column in HPLC coupled with a diode-array detector, was developed for the quantitative determination of benzodiazepines in whole blood. The present method has been applied to the ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2004.01.023

    authors: Bugey A,Staub C

    更新日期:2004-05-28 00:00:00

  • Isothermal titration calorimetry study of epicatechin binding to serum albumin.

    abstract::The interaction of epicatechin with bovine serum albumin (BSA) was studied by isothermal titration calorimetry. The binding constant (K) and associated thermodynamic binding parameters (n, DeltaH) were determined for the interaction at three solution concentrations of BSA using a binding model assuming independent bin...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2006.02.004

    authors: Frazier RA,Papadopoulou A,Green RJ

    更新日期:2006-08-28 00:00:00

  • A stability-indicating HPLC assay method for docetaxel.

    abstract::A novel stability-indicating high-performance liquid chromatographic assay method was developed and validated for docetaxel in the presence of degradation products generated from forced decomposition studies. A gradient HPLC method was developed to separate the drug from the degradation products, using a Hichrom RPB H...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2006.01.011

    authors: Rao BM,Chakraborty A,Srinivasu MK,Devi ML,Kumar PR,Chandrasekhar KB,Srinivasan AK,Prasad AS,Ramanatham J

    更新日期:2006-05-03 00:00:00