Critical evaluation of methods for end-point determination in pharmaceutical blending processes

Blanco, M.; Cueva-Mestanza, R.; Cruz, Jordi

doi:10.1039/c2ay25379h

Cited by 17 publications

(8 citation statements)

References 52 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The MBSD method is straightforward and easily implemented, but provides inaccurate predictions owing to its poor sensitivity for identifying the blending end-point as a result of the strong effects of spectral variation and noise. 12 , 23 The PC-SDA method provided results on a par with those of the PLS method; like MBSD, however, it is subject to the deleterious effects of spectral variations and noise [ Figure 4(f)]. In contrast, the PC-SDA method requires no reference and its threshold is statistically calculated and, hence, reproducible.…”

Section: Pls Calibration Methodsmentioning

confidence: 99%

Assessment of Chemometric Methods for the Non-Invasive Monitoring of Solid Blending Processes Using Wireless near Infrared Spectroscopy

Rosas

Blanco

Santamaría

et al. 2013

Journal of Near Infrared Spectroscopy

View full text Add to dashboard Cite

The US Food and Drug Administration's process analytical technology (PAT) initiative has encouraged the pharmaceutical industry to strengthen research with a view to developing new analytical technologies for improving blending processes. Near infrared (NIR) spectroscopy, which is sensitive to both physical and chemical attributes of substances, has proved a powerful non-invasive analytical technique for this purpose. In this paper, we propose a criterion to assess blending uniformity and accurately detect the end-point of a blending process. The criterion was established by using partial least squares (PLS) regression and calibration-free methods including moving block standard deviation of spectra, principal component scores distance analysis and the mixing index (M). The mixing index was found to provide accurate, robust results with a view to assessing blending uniformity, as was PLS for detecting blending endpoints. This novel criterion allowed us to assess the homogeneity of a mixture, without the need of a reference method, a golden batch or a calibration set. In fact, the M index was found to be an easy method and it is a highly suitable tool for PAT as it allows the accurate, precise real-time monitoring of blending processes with minimal intervention of the analyst.

show abstract

Section: Pls Calibration Methodsmentioning

confidence: 99%

Assessment of Chemometric Methods for the Non-Invasive Monitoring of Solid Blending Processes Using Wireless near Infrared Spectroscopy

Rosas

Blanco

Santamaría

et al. 2013

Journal of Near Infrared Spectroscopy

View full text Add to dashboard Cite

show abstract

“…In this study, three consecutive spectra based on all wavelengths were used, while one spectrum was moved at a time. The detailed computing formula for MBSD can be found in the relevant reference [13] .…”

Section: Multivariate Modelingmentioning

confidence: 99%

In-line spectroscopy combined with multivariate analysis methods for endpoint determination in column chromatographic adsorption processes for herbal medicine

Jiang

2022

Acupuncture and Herbal Medicine

View full text Add to dashboard Cite

Objective: In a chromatographic cycle, the adsorption process is a critical unit operation that has a significant impact on downstream processes and, ultimately, the quality of the final products. The development of a rapid method to determine the endpoints of adsorption processes in a large-scale manufacturing is of substantial importance for herbal medicine (HM) manufacturers.Methods: In this study, the adsorption of saponins on a macroporous resin column chromatograph, a critical unit operation in Panax notoginseng (Burkill) F.H.Chen injection manufacturing, was considered as an example. The evaluation results of in-line ultraviolet and visible spectra combined with various multivariate analysis methods, including the moving block standard deviation (MBSD), difference between the moving block average and the target spectrum (DMBA-TS), soft-independent modeling of class analogy (SIMCA), and partial least-squares discriminant analysis (PLS-DA), were compared.Results: MBSD was unsuitable for adsorption processes. The relative standard errors of prediction between the predicted and experimental endpoints were 13.2%, 4.67%, and 5.71% using DMBA-TS, SIMCA, and PLS-DA, respectively.Conclusions: Among the considered analysis methods, SIMCA and PLS-DA were more effective for endpoint determination. The results of this study provide a more comprehensive overview of the effectiveness of various multivariate analysis methods to facilitate the selection of the most suitable method. This study was also conducive to address the issues of the in-line detection of adsorption endpoints to guide practical HM manufacturing.

show abstract

“…Mixing time has been assessed for different blending processes: for instance, NIR probes were applied to a modified V-blender (Sekulic et al, 1996), a Nauta mixer (Berntsson et al, 2002) and a lab-scale blender (Blanco et al, 2002). Further applications can be found in the work of Blanco, Cueva-Mestanza et al (2012) which provided a good review of blending time assessment and a detailed comparison of the different methods and pre-treatments. Given the great success of NIR in estimating the end time of powder blending, this technique was also employed to monitor and determine the end time of other processes.…”

Section: A C C E P T E D Accepted Manuscriptmentioning

confidence: 99%

Towards online Near-Infrared spectroscopy to optimise food product mixing

Barone¹,

Glassey²,

Montague³

2019

Journal of Food Engineering

View full text Add to dashboard Cite

This paper advances the use of in-situ Near-Infrared (NIR) spectroscopy as the basis for an in-line control system to optimise mixing time of food powder blends. A non-contact NIR fibre-optic probe installed in a conical screw mixer was used to scan three powder mixtures characterised by different particle size distribution and component distribution. The current state of the art is extended by comparing Conformity Index and Standard deviation of the Moving Block Standard Deviation (MBSD), establishing the optimal pre-treatment combination and investigating the effects of the mixture properties on the results. Products with a broad particle size distribution were more accurately represented using derivatives rather than SNV and Detrending, while products with a broad component distribution showed good results with all pre-treatments. This study evaluated the effect of data pre-treatments on mixing time for different physical properties of powder blends and provided a general guidance on the most appropriate pre-treatment.

show abstract

Critical evaluation of methods for end-point determination in pharmaceutical blending processes

Cited by 17 publications

References 52 publications

Assessment of Chemometric Methods for the Non-Invasive Monitoring of Solid Blending Processes Using Wireless near Infrared Spectroscopy

Assessment of Chemometric Methods for the Non-Invasive Monitoring of Solid Blending Processes Using Wireless near Infrared Spectroscopy

In-line spectroscopy combined with multivariate analysis methods for endpoint determination in column chromatographic adsorption processes for herbal medicine

Towards online Near-Infrared spectroscopy to optimise food product mixing

Contact Info

Product

Resources

About