Development and validation of a ultra-high-performance liquid chromatography-UV method for the detection and quantification of erectile dysfunction drugs and some of their analogues found in counterfeit medicines

Sacré, Pierre-Yves; Deconinck, Éric; Chiap, Patrice; Crommen, Jacques; Mansion, François; Rozet, Eric; Courselle, P.; Beer, Jacques O. De

doi:10.1016/j.chroma.2011.07.029

Cited by 48 publications

(20 citation statements)

References 37 publications

(11 reference statements)

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“…The flow was 1 mL/min; the column temperature was set at 30 °C; the sample temperature was set at 15 °C and detection was performed at a wavelength of 254 nm. For the samples containing sildenafil citrate the injection volume was set at 5 µL, while for the tadalafil-containing samples it was set at 20 µL [17] .…”

Section: Methodsmentioning

confidence: 99%

Comparative dissolution study on counterfeit medicines of PDE-5 inhibitors

Deconinck

Andriessens

Bothy

et al. 2014

Journal of Pharmaceutical Analysis

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Counterfeit medicines are a growing problem in both developing and industrialised countries. In general the evaluation of these medicines is limited to the identification and the dosage of the active ingredients. In this study in vitro dissolution tests were conducted on two sets of counterfeit medicines containing PDE-5 inhibitors (sildenafil citrate and tadalafil). The dissolution profiles were statistically compared to the ones of the genuine products using the f2-method and a comparison at each time point using the Cochran test.The results showed low equivalences between counterfeit and genuine products as well as higher variations around the mean dissolution value at the different time points for the counterfeit products.

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Section: Methodsmentioning

confidence: 99%

Comparative dissolution study on counterfeit medicines of PDE-5 inhibitors

Deconinck

Andriessens

Bothy

et al. 2014

Journal of Pharmaceutical Analysis

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“…Liquid chromatography (LC), namely HPLC and more recently ultra‐high‐performance LC (UHPLC), is the most commonly reported separation technique applied for the analysis of pharmaceutical adulterants in dietary supplements, in particular those used for weight loss and sexual performance enhancement (Table and ). The use of HPLC coupled to ultraviolet detection, especially HPLC with a diode array detector (DAD), has been recognized for the preliminary identification and screening of adulterants in weight‐loss products (De Cock and others ; De Carvalho and others ; Deconinck and others ; Rebiere and others ; Csupor and others ) and sexual PEDs (Singh and others ; Ortiz and others ; Savaliya and others ; Sacré and others ; Venhuis and others , 2011b; Wollein and others ; Jankovics and others ; Fejos and others ; Zhang and others ). HPLC‐UV has also been used in semipreparative chromatography for unknown compounds isolation purposes (Lee and others ).…”

Section: Determination Of Adulterating Substancesmentioning

confidence: 99%

Adulteration of Dietary Supplements by the Illegal Addition of Synthetic Drugs: A Review

Rocha

Amaral

Oliveira

2015

Comp Rev Food Sci Food Safe

184

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In the last few years, the consumption of dietary supplements, especially those having plants as ingredients, has been increasing due to the common idea that they are natural products posing no risks to human health. In the European Union and the United States, dietary supplements are legally considered as foods/special category of foods, thus are not being submitted to any safety assessment prior to their commercialization. Among the issues that can affect safety, adulteration by the illegal addition of pharmaceutical substances or their analogs is of major concern since unscrupulous producers can falsify these products to provide for quick effects and to increase sales. This review discusses the various classes of synthetic drugs most frequently described as being illegally added to dietary supplements marketed for weight loss, muscle building/sport performance and sexual performance enhancement. Information regarding regulation and consumption is also presented. Finally, several conventional and advanced analytical techniques used to detect and identify different adulterants in dietary supplements and therefore also in foods, with particular emphasis on plant food supplements, are critically described. This review demonstrates that dietary supplement adulteration is an emerging food safety problem and that an effective control by food regulatory authorities is needed to safeguard consumers.

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“…Several parameters were considered critical factors for the analysis. The self-imposed parameter limits set in for these parameters were inspired by other publications (6)(7)18) and own experience. Parameters were studied as follows: The flow of the mobile phase (± 2 %), column temperature (± 5 °C), buffer strength of the aqueous component (± 5 mM) and pH value (± 0.25) for both mobile phase A and mobile phase B were investigated by injecting a series of dilutions with three individual standards for lowest, medium and highest concentrations (of the concentration range discussed in the previous section) of levodopa, carbidopa, benserazide and entacapone in triplicate.…”

Section: Analytical Methods Validationmentioning

confidence: 99%

Development and Validation of a Robust and Efficient HPLC Method for the Simultaneous Quantification of Levodopa, Carbidopa, Benserazide and Entacapone in Complex Matrices

Wollmer

Klein

2017

J Pharm Pharm Sci

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-Purpose:A variety of fixed-dose combination products is used in the therapy of Parkinson Disease. However, to date a proper analytical method applicable for comparative screening of different antiparkinson products was not available. The objective of the present work was thus to develop and validate an analytical method for the simultaneous quantification of levodopa, carbidopa, benserazide and entacapone. The method should be applicable for quantifying samples from drug release experiments with marketed products and prototype formulations performed under compendial and biorelevant test conditions. Methods: A fast and robust method applicable for separation and quantification of the four compounds was developed and validated according to International Conference on Harmonization guidelines. Method validation covered applicability to a wide concentration range of all compounds and peak separation in complex sample matrices such as biorelevant dissolution media. Results: The compounds were successfully separated by using a gradient elution method on an endcapped LiChrospher 100 RP-18 (250 x 4.6 mm, 5 µm) column coupled with a LiChrospher 100 RP-18 precolumn (4 x 4 mm, 5 µm) at a column temperature of 35.0 °C and a flow rate of 1.50 mL/min. The injection volume was 30 µL and the detection wavelengths were 280 and 210 nm, respectively. For all drug/media combinations the method was linear (r 2 > 0.999) for a concentration range corresponding to 1.25 -125 % label claim (i.e. 200 mg levodopa/entacapone and 50 mg carbidopa/benserazide) released. All other validation parameters were in the specified limits over the same concentration range. Conclusion: The new method allows for robust and fast separation of levodopa, carbidopa, benserazide and entacapone without any interference caused by excipients or ingredients of compendial and biorelevant dissolution media and thus presents a valuable tool in both formulation development and in vitro drug release screening of numerous fixed-dose combinations of antiparkinson drugs.

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Development and validation of a ultra-high-performance liquid chromatography-UV method for the detection and quantification of erectile dysfunction drugs and some of their analogues found in counterfeit medicines

Cited by 48 publications

References 37 publications

Comparative dissolution study on counterfeit medicines of PDE-5 inhibitors

Comparative dissolution study on counterfeit medicines of PDE-5 inhibitors

Adulteration of Dietary Supplements by the Illegal Addition of Synthetic Drugs: A Review

Development and Validation of a Robust and Efficient HPLC Method for the Simultaneous Quantification of Levodopa, Carbidopa, Benserazide and Entacapone in Complex Matrices

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