Ion Beam Analysis and PD-MS As New Analytical Tools for Quality Control of Pharmaceuticals: Comparative Study from Fluphenazine in Solid Dosage Forms

Abstract

In order to evaluate the potential of accelerator based analytical techniques ((particle induced X-ray emission (PIXE), particle induced gamma-ray emission (PIGE), and particle desorption mass spectrometry (PD-MS)) for the analysis of commercial pharmaceutical products in their solid dosage form, the fluphenazine drug has been taken as a representative example. It is demonstrated that PIXE and PIGE are by far the best choice for quantification of the active ingredient (AI) (certification with 7% precision) from the reactions induced on its specific heteroatoms fluorine and sulfur using pellets made from original tablets. Since heteroatoms cannot be present in all types of drugs, the PD-MS technique, which makes easily the distinction between AI(s) and excipients, has been evaluated for the same material. It is shown that the quantification of AI is obtained via the detection of its protonated molecule. However, calibration curves have to be made from the secondary ion yield variations since matrix effects of various nature are characteristics of such mixtures of heterogeneous materials (including deposits from soluble components). From the analysis of solid tablets, (either transformed into pellets and even as received), it is strongly suggested that the physical state of the grains in the mixture is a crucial parameter in the ion emission and accordingly for the calibration curves. As a result of our specific (but not optimized) conditions the resulting precision is <17% with an almost linear range extending from 0.04 to 7.87 mg of AI in a tablet made under the manufacturer conditions (the commercial drug product is labeled at 5 mg).

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

“…119 Both PIXE and PIGE were shown to be excellent techniques for the quantitation of active ingredients containing heteroatoms in solid tablets. Nsouli and colleagues have evaluated these techniques for the analysis of commercially available pharmaceutical products, including fluphenazine (an anti-psychotic drug containing S and F atoms), in their solid form.…”

“…Nsouli and colleagues have evaluated these techniques for the analysis of commercially available pharmaceutical products, including fluphenazine (an anti-psychotic drug containing S and F atoms), in their solid form. 119 Both PIXE and PIGE were shown to be excellent techniques for the quantitation of active ingredients containing heteroatoms in solid tablets. However, since not all active ingredients contain heteroatoms, the use of PD-MS was evaluated as a means of determining active ingredients in the presence of excipients in the tablets.…”

MIL88-A as a mediator for the degradation of sulfamethoxazole in PS systems: implication of solar irradiation for process improvement

“…For example, we investigated the combination of PS activators in systems such as UVA/MIL88-A/PS or solar/MIL88-A/PS and monitored the impact on SMX removal in terms of degradation rate and transformation products nature and persistence. This was possible upon using the time of flight secondary ion mass spectrometry (ToF SIMS) technique previously used for the characterization of materials of environmental and pharmaceutical interests [59][60][61][62][63] as well as the Time of Flight high…”

“…For example, we investigated the combination of PS activators in systems such as UVA/MIL88-A/PS or solar/MIL88-A/PS and monitored the impact on SMX removal in terms of the degradation rate and transformation product nature and persistence. This was possible upon using the time of ight secondary ion mass spectrometry (ToF SIMS) technique previously used for the characterization of materials of environmental and pharmaceutical interest [59][60][61][62][63] as well as the time of ght high resolution mass spectrometry (ToF HRMS) technique for the identication of transformation products. Moreover, we studied the effect of various factors such as salinity, carbonates, and phosphates on the performance of both systems UVA/MIL88-A/ PS/SMX and solar/MIL88-A/PS/SMX toward SMX degradation and the potential application of this system on real pharmaceutical industry effluents.…”

Determination of fluorine concentrations in soil samples using proton induced gamma-ray emission

“…PIGE is sensitive technique for low Z elements (Z \ 17) especially for lithium and fluorine [10,11]. It finds applications in many fields including pharmaceuticals [11], glass [12], teeth [13,14], aerosols [15] and geological and environmental reference materials [16,17]. This makes it complementary to techniques like particle induced X-ray emission (PIXE), X-ray fluorescence (XRF) and neutron activation analysis (NAA).…”