The critical role of NIR spectroscopy and statistical process control (SPC) strategy towards captopril tablets (25 mg) manufacturing process understanding: a case study

Abstract

In this work, near-infrared spectroscopy (NIRS) method was used to evaluate the uniformity of dosage units of three captopril 25 mg tablets commercial batches. The performance of the calibration method was assessed by determination of Q value (0.9986), standard error of estimation (C-set SEE = 1.956), standard error of prediction (V-set SEP = 2.076) as well as the consistency (106.1%). These results indicated the adequacy of the selected model. The method validation revealed the agreement of the reference high pressure liquid chromatography (HPLC) and NIRS methods. The process evaluation using the NIRS method showed that the variability was due to common causes and delivered predictable results consistently. Cp and Cpk values were, respectively, 2.05 and 1.80. These results revealed a non-centered process in relation to the average target (100% w/w), in the specified range (85-115%). The probability of failure was 21:100 million tablets of captopril. The NIRS in combination with the method of multivariate calibration, partial least squares (PLS) regression, allowed the development of methodology for the uniformity of dosage units evaluation of captopril tablets 25 mg. The statistical process control strategy associated with NIRS method as PAT played a critical role in understanding of the sources and degree of variation and its impact on the process. This approach led towards a better process understanding and provided the sound scientific basis for its continuous improvement.

Statistical process control of manufacturing tablets for antiretroviral therapy

“…When it is between 1.34 and 1.99, the process is considered suitable; values between 1.0 and 1.33 show that the process requires corrective action, and values less than 1.0 denote a non-capable process. If it is equal to 1.0, then 99.73 % of the values lie within the specification limits (Dal Curtivo et al, 2015). Thus, 0.27 % of the units manufactured may be out of specification (example: in 1,000,000 units manufactured, 2,700 units OOS).…”

“…Cp and Cpk were 1. 43 and 1.27 and 1.69 and 1.83, respectively (de Souza Botelho et al, 2011;Dal Curtivo et al, 2015).…”

Evaluation of temperature compensation methods for a near‐infrared calibration to predict the viscosity of micellar liquids

“…Near‐infrared (NIR) spectroscopy has proven to be a successful analytical tool in measuring chemical and physical properties in‐line due to its non‐destructive nature, speed of analysis and ease of implementation in manufacturing environments 1–9 . Though NIR spectroscopy has low selectivity, it can be combined with multivariate modelling techniques such as principal component analysis (PCA) or partial least squares (PLS) to extract the relevant information and develop predictive models.…”