HPLC for in-process control in the production of sultamicillin

A fast HPLC method has been developed for simultaneous determination of sultamicillin and its synthesis precursors. The analytes are separated in 2.5 min by means of a Kromasil 100 C18 column (50 mm Â 2.1 mm i.d., 3.5 mm) at 25 C. The mobile phase (A: 5 mM KH 2 PO 4 and 20 mM KCl adjusted to pH 6.0 with H3PO4 plus 1% THF and B: acetonitrile with 1% THF) was pumped at a flow rate of 0.5 mL min À1 according to the fast gradient mode: 0-0.9 min, 40% B; 0.9-1.0 min, 85% B; 1.0-2.5 min, 85% B; 2.5-2.6 min, 40% B, 2.6-4.0 min, 40% B. Detection was by ultraviolet absorbance at 205 nm. The method was validated in accordance with the International Conference on Harmonisation (ICH) guidelines, good accuracy, intermediate precision ( 3.8%), and linearity being observed for all compounds. This method is sensitive (limits of detection ranged between 0.1-1.1 mg l À1 ) and selective for quantifying sultamicillin and its synthesis precursors and could be used for in-process control.

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“…Only one article concerning the in-process control of sultamicillin has been published, [34] but it makes use of classical HPLC.…”

Section: Introductionmentioning

confidence: 99%

High Speed Liquid Chromatography for In-Process Control of Sultamicillin

Gomis

Núñez

Enguita

et al. 2008

Journal of Liquid Chromatography & Related Technologies

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“…Currently, many offline technologies and strategies (e.g., high-performance liquid chromatography [HPLC], mass spectrometry [MS], and ultraviolet [UV] spectrophotometry) are used in IPC for quality analysis of pharmaceutical medications. − However, such technologies are generally used for API monitoring and are time-consuming, tedious, and often destructive in nature. , Hence, more rapid and accurate techniques are needed for real-time testing and validation of the final product. Moreover, rapid control of the manufacturing process using process analytical technology (PAT), promoted by the Food and Drug Administration (FDA), provides important opportunities for improving our understanding and control of the process while decreasing safety risks associated with sampling and testing. , …”

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confidence: 99%

In-Process Control Assay of Pharmaceutical Microtablets Using Hyperspectral Imaging Coupled with Multivariate Analysis

et al. 2016

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Monitoring the amount of active pharmaceutical ingredient (API) in finished dosage form is important to ensure the content uniformity of the product. In this report, we summarize the development and validation of a hyperspectral imaging (HSI) technique for rapid in-line prediction of the active pharmaceutical ingredient (API) in microtablets with concentrations varying from 60 to 130% API (w/w). The tablet spectra of different API concentrations were collected in-line using an HSI system within the visible/near-infrared (vis/NIR; 400-1000 nm) and short-wave infrared (SWIR; 1100-2500 nm) regions. The ability of the HSI technique to predict the API concentration in the tablet samples was validated against a reference high-performance liquid chromatography (HPLC) method. The prediction efficiency of two different types of multivariate data modeling methods, that is, partial least-squares regression (PLSR) and principle component regression (PCR), were compared. The prediction ability of the regression models was cross-validated against results generated with the reference HPLC method. The results obtained from the PLSR models showed reliable performance for predicting the API concentration in SWIR region. The highest coefficient of determination (Rp) was 0.96, associated with the lowest predicted error and bias of 4.45 and -0.35%, respectively. Furthermore, the concentration-mapped images of PLSR and PCR models were used to visually characterize the API concentration present on the tablet surface. Based on these results, we suggest that HSI measurement combined with multivariate data analysis and chemical imaging could be implemented in the production environment for rapid in-line determination of pharmaceutical product quality.

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