A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives

Monge, Marı́a Eugenia; Dwivedi, Prabha; Zhou, Manshui; Payne, Michael; Harris, C. Wilson; House, Blaine; Juggins, Yvonne; Cizmarik, Peter; Newton, Paul N.; Fernández, Facundo M.; Jenkins, David W.

doi:10.1371/journal.pone.0095353

Cited by 15 publications

(12 citation statements)

References 19 publications

(20 reference statements)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Samples of genuine and fake levonorgestrel tablets (0.75 mg and 1.5 mg) were kindly provided by Paul N. Newton (Centre for Tropical Medicine, Churchill Hospital, University of Oxford, UK) and Dr. David Jenkins (FHI 360, USA), respectively. The content of the samples was previously verified at the Georgia Institute of Technology using multiple analytical platforms including DART and ESI‐MS/MS with and without liquid chromatography (LC) separation and 2D DOSY 1 H NMR spectroscopy . Dried blood spots, spiked with chloroquine, on Whatman filter paper were kindly provided by Dr. Michael D. Green (Center for Disease Control and Prevention (CDC), Atlanta, GA, USA).…”

Section: Methodsmentioning

confidence: 99%

“…The content of the samples was previously verified at the Georgia Institute of Technology using multiple analytical platforms including DART and ESI-MS/MS with and without liquid chromatography (LC) separation and 2D DOSY 1 H NMR spectroscopy. [30] Dried blood spots, spiked with chloroquine, on Whatman filter paper were kindly provided by Dr. Michael D. Green (Center for Disease Control and Prevention (CDC), Atlanta, GA, USA). Chloroquine diphosphate salt (powder, purity ≥98%) used as standard was purchased from Sigma-Aldrich.…”

Section: Methodsmentioning

confidence: 99%

See 1 more Smart Citation

Desorption atmospheric pressure photoionization and direct analysis in real time coupled with travelling wave ion mobility mass spectrometry

Räsänen

Dwivedi

Fernández

et al. 2014

Rapid Comm Mass Spectrometry

Self Cite

View full text Add to dashboard Cite

RATIONALE: Ambient mass spectrometry (MS) is a tool for screening analytes directly from sample surfaces. However, background impurities may complicate the spectra and therefore fast separation techniques are needed. Here, we demonstrate the use of travelling wave ion mobility spectrometry in a comparative study of two ambient MS techniques. METHODS: Desorption atmospheric pressure photoionization (DAPPI) and direct analysis in real time (DART) were coupled with travelling wave ion mobility mass spectrometry (TWIM-MS) for highly selective surface analysis. The ionization efficiencies of DAPPI and DART were compared. Test compounds were: bisphenol A, benzo[a]pyrene, ranitidine, cortisol and α-tocopherol. DAPPI-MS and DART-TWIM-MS were also applied to the analysis of chloroquine from dried blood spots, and α-tocopherol from almond surface, and DAPPI-TWIM-MS was applied to analysis of pharmaceuticals and multivitamin tablets. RESULTS: DAPPI was approximately 100 times more sensitive than DART for bisphenol A and 10-20 times more sensitive for the other compounds. The limits of detection were between 30-290 and 330-8200 fmol for DAPPI and DART, respectively. Also, from the authentic samples, DAPPI ionized chloroquine and α-tocopherol more efficiently than DART. The mobility separation enabled the detection of species with low signal intensities, e.g. thiamine and cholecalciferol, in the DAPPI-TWIM-MS analysis of multivitamin tablets. CONCLUSIONS: DAPPI ionized the studied compounds of interest more efficiently than DART. For both DAPPI and DART, the mobility separation prior to MS analysis reduced the amount of chemical noise in the mass spectrum and significantly increased the signal-to-noise ratio for the analytes.

show abstract

Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Desorption atmospheric pressure photoionization and direct analysis in real time coupled with travelling wave ion mobility mass spectrometry

Räsänen

Dwivedi

Fernández

et al. 2014

Rapid Comm Mass Spectrometry

Self Cite

View full text Add to dashboard Cite

show abstract

“…There are probably thousands of "Third Men" hidden in today's world-for example, a Parisian who manufactured falsified antimalarials containing laxatives, 16 international trade from India, 17 and emergency contraceptives containing antimalarials in South America. 18 There are also many cases of substandard medicines-poor quality medicines produced through negligence, sometimes gross, in the manufacturing processes but not deliberately designed to defraud patients and heath systems. 19 Substandard anti-infective drugs often contain less than the stated amount of active ingredient and are therefore likely to be under-recognised drivers of antimicrobial resistance.…”

Section: Illegal Trade Continues Todaymentioning

confidence: 99%

Fake penicillin,The Third Man,and Operation Claptrap

Newton

Timmermann²

2016

BMJ

View full text Add to dashboard Cite

“…Screening will reduce the number of samples that must be processed by a central QC laboratory which will in turn reduce costs and reduce the time delays for the patient's treatment. There have been several approaches to develop suitable screening systems including the Minilab™ based on TLC test methods [16], a handheld Raman Spectroscopy device [5] and systems based on Near Infrared Spectroscopy (NIR) [17]. The Minilab™ requires training in handling chemicals and the test sample has to be solvent extracted prior to analysis which increases both the time and complexity of each test.…”

Section: Introductionmentioning

confidence: 99%

Counterfeit Tablet Investigations: Can ATR FT/IR Provide Rapid Targeted Quantitative Analyses?

Lawson¹

2014

J Anal Bioanal Tech

View full text Add to dashboard Cite

Counterfeit medicines are now a global public health problem. In developed countries up to 1% of medicines are reported to be counterfeit whilst in developing countries the level is ~30-40%. In this research the potential of Attenuated Total Reflection (ATR) FT/IR techniques to provide rapid quantitative analyses of suspect tablet formulations is reported. Unlike conventional tablet analyses where several tablets are crushed and solvent extracted, ATR FT/IR methods require that only a single tablet be crushed prior to analysis. This provides a considerable time saving over the solvent extraction protocols cited in the British Pharmacopoeia. Reference ATR FT/IR spectra of the active pharmaceutical ingredient (API) and excipients, from crushed tablets, were recorded for identification purposes. Quantitative data was obtained from ATR FT/IR spectra of calibrated mixtures of the API in the excipients. Tablet samples from various countries, India, Africa, China, Belgium and the UK were examined. Initial results showed the API could be identified down to ca 5% w/w of the tablet. Quantification was linear with selected characteristic peak areas for each API/excipient mixture. The analysis of the tablet samples generally showed good agreement with expectation. This was confirmed by conventional extractive analyses followed by UV quantification. ATR FT/IR can therefore identify counterfeit tablets rapidly without the need for solvents. Whilst LC-MS/MS and NMR techniques may be the 'gold standards' of the analytical world they are of much reduced value in sub-Saharan African countries whereas a portable ATR FT/IR may prevent the use of counterfeit antimalarial tablets and contribute to improvements in patient health.

show abstract

A Tiered Analytical Approach for Investigating Poor Quality Emergency Contraceptives

Cited by 15 publications

References 19 publications

Desorption atmospheric pressure photoionization and direct analysis in real time coupled with travelling wave ion mobility mass spectrometry

Desorption atmospheric pressure photoionization and direct analysis in real time coupled with travelling wave ion mobility mass spectrometry

Fake penicillin,The Third Man,and Operation Claptrap

Counterfeit Tablet Investigations: Can ATR FT/IR Provide Rapid Targeted Quantitative Analyses?

Contact Info

Product

Resources

About