Detection of falsified clopidogrel in the presence of excipients using voltammetry

Shergill, Ricoveer Singh; Kristová, Petra; Patel, Bhavik Anil

doi:10.1039/d1ay01602d

Cited by 2 publications

(3 citation statements)

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“…These results indicate that measurements of melatonin tablets can be conducted in the presence of the excipients and thus reduce the need for extra sample preparation steps allowing for total analysis. Our findings are identical to other studies which have shown that electrochemical measurements can be conducted in particulate solutions [38][39][40]. Given our ability to clearly detect the presence of melatonin within the tablet without additional sample preparation steps, we conducted a calibration response in the presence of excipients.…”

Section: Analytical Performance Of the 3d-printed Pestle And Mortar F...supporting

confidence: 82%

“…Calibrations were conducted in the concentration range of 300 to 37.5 µg/mL. This approach was taken as we have previously shown that tablet excipients can reduce the current response of melatonin and other pharmaceutical active ingredients [38][39][40]. To evaluate the stability for repeated measurements of melatonin tablets, five repeated measurements were conducted using melatonin tablets.…”

Section: Electrochemical Measurements Using the Pestle And Mortarmentioning

confidence: 99%

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3D-printed electrochemical pestle and mortar for identification of falsified pharmaceutical tablets

et al. 2022

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Falsified medicines and healthcare supplements provide a major risk to public health and thus early identification is critical. Although a host of analytical approaches have been used to date, they are limited, as they require extensive sample preparation, are semiquantitative and/or are inaccessible to low-and middle-income countries. Therefore, for the first time we report a simple total analysis system which can rapidly and accurately detect falsified medicines and healthcare supplements. We fabricated a poly-lactic acid (PLA) pestle and mortar and using a commercial 3D printer, then made carbon black/PLA (CB/PLA) electrodes in the base of the mortar using a 3D printing pen to make an electrochemical cell. The pestle and mortar were able to crush and grind the tablets into a fine powder to the same consistency as a standard laboratory pestle and mortar. Using 2 melatonin tablets to characterise the device, the 3D printed pestle and mortar was able to detect the concentration of melatonin in the presence of insoluble excipients. The calibration plot showed a linear response from 37.5 to 300 µg/mL, where the limit of detection was 7 µg/mL. Electrochemical treatment was able to regenerate the CB/PLA working electrode allowing for repeated use of the device. In a blinded study, the device was able to accurately determine falsified melatonin tablets with recovery percentages between 101 and 105 %. This was comparable to HPLC. Overall, these findings highlight that our 3D printed electrochemical pestle and mortar is an accessible and effective total analysis system that can have the ability to identify falsified medicines and healthcare supplements in remote locations.

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Section: Analytical Performance Of the 3d-printed Pestle And Mortar F...supporting

confidence: 82%

Section: Electrochemical Measurements Using the Pestle And Mortarmentioning

confidence: 99%

3D-printed electrochemical pestle and mortar for identification of falsified pharmaceutical tablets

et al. 2022

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“…There are several methods reported in the literature for the analysis of clopidogrel bisulfate 5 , such as UV/Vis spectrophotometry, high-performance liquid chromatography (HPLC), micellar liquid chromatography (MLC), micellar electrokinetic chromatography (MEKC), high-performance thin layer chromatography (HPTLC), and liquid chromatography-tandem mass spectrometry (LC-MS/MS) 6 . Also, electrochemical methods were used for the analysis of clopidogrel bisulfate [7][8][9] .…”

Section: Introductionmentioning

confidence: 99%

Development and Validation of RP-HPLC Method for Analysis of Counterfeit Clopidogrel

Soliman,

Mohamed Mabrouk,

Hammad

et al. 2024

Journal of Advanced Medical and Pharmaceutical Research

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The isocratic RP-HPLC method was developed and validated for the analysis of clopidogrel bisulfate counterfeited with acetyl salicylic acid and applied for the determination of clopidogrel bisulfate in pharmaceutical dosage forms. Clopidogrel bisulfate is commonly counterfeited with acetyl salicylic acid and it is not labeled to contain acetyl salicylic acid due to their similar pharmacological effect in inhibiting platelet aggregation. The mobile phase was composed of potassium dihydrogen phosphate buffer 0.02M (pH 2.8) and methanol 30:70 (v/v). The flow rate was 1.5mL/min. The Diode array detector was set at 220 nm. The linearity ranges were 10-70 µg/mL and 6-50 µg/mL for clopidogrel bisulfate and acetyl salicylic acid, respectively. The retention time was 2.5 min and 10.23 min for clopidogrel bisulfate and acetyl salicylic acid, respectively. The method was validated according to ICH guidelines. The developed method was successfully applied for the determination of clopidogrel bisulfate counterfeited with acetyl salicylic acid as well as the estimation of clopidogrel bisulfate in its different dosage forms.

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Detection of falsified clopidogrel in the presence of excipients using voltammetry

Abstract: There has been a recent surge in the amount of substandard and falsified clopidogrel. Pharmacopeial based assays using high performance liquid chromatograph and mass spectroscopy are widely used for measurement...

Cited by 2 publications

References 31 publications

3D-printed electrochemical pestle and mortar for identification of falsified pharmaceutical tablets

3D-printed electrochemical pestle and mortar for identification of falsified pharmaceutical tablets

Development and Validation of RP-HPLC Method for Analysis of Counterfeit Clopidogrel

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