Quantitative Application of in Situ ATR-FTIR and Raman Spectroscopy in Crystallization Processes

Cornel, Jan H.; Lindenberg, Christian; Mazzotti, Marco

doi:10.1021/ie800236v

Cited by 132 publications

(177 citation statements)

References 41 publications

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“…The Cornel et al 28) reported that the multivariate calibration approach was applicable to Raman spectroscopy for multiphase and multicomponent dynamic processes such as solventmediated polymorphic transformation. Multivariate analysis can estimate solute concentration even from weak signals in Raman spectrum.…”

Section: Quantitative Analysis Of Pharmaceutical Bulk Powders By Pls mentioning

confidence: 99%

Quantification of Pharmaceutical Compounds Based on Powder X-Ray Diffraction with Chemometrics

Otsuka

Itô

Matsumura

et al. 2016

CHEMICAL & PHARMACEUTICAL BULLETIN

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We propose an approach for the simultaneous determination of multiple components in pharmaceutical mixed powder based on powder X-ray diffraction (PXRD) method coupled with chemometrics. Caffeine anhydrate, acetaminophen and lactose monohydrate were mixed at various ratios. The samples were analyzed by PXRD method in the ranges of 2θ 5.00-30.0 and 35.0-45.0 degrees. Obtained diffractograms were analyzed by conventional peak intensity method, multi curve resolution (MCR)-alternating least squares (ALS) method and partial least squares (PLS) method. Constructed PLS models can most accurately predict the concentrations among different methods used. Each regression vector of PLS correlates not only to the compound of interest but also to the coexisting compounds. The combination of PXRD and PLS methods is concluded to be powerful approach for analyzing multi components in pharmaceutical formulations.Key words powder X-ray diffraction; partial least square; pharmaceutical formulationThe polymorphs and pseudo-polymorphs (hydrates and solvates) of pharmaceuticals exhibit different physicochemical properties such as solubility, dissolution rate, stability and hygroscopicity. These properties strongly relate to the pharmaceutical properties in their dosage forms such as specific bioavailability, efficacy, stability and toxicity.1) Pharmaceutical regulations are, therefore, required for producing appropriate bulk drugs, the crystalline modifications of which (i.e., polymorphism) are well specified or precisely controlled. 2)Powder X-ray diffraction (PXRD) analysis is the most frequently used method for identifying crystalline modifications and for determining their contents in bulk powders.3) Any crystals have their own PXRD patterns. Pharmaceutical formulations are, in general, composed of multiple components including excipients. PXRD is, therefore, useful to identify crystalline compounds in the formulation and to determine their amounts in a non-contact and non-destructive fashion. 4,5) However, PXRD method has large relative errors, typically around ±5%. Such shortcoming of PXRD method is serious when two or more components having broad and overlapping X-ray diffraction peaks are contained in one formulation.Regulatory authorities such as the U.S. Food and Drug Administration and the International Conference on Harmonization have requested to use Process Analytical Technology (PAT) in order to reduce the production risk of inferior pharmaceuticals.6) Since the introduction of guidelines for PAT, online and real-time analysis have increasingly been accepted in pharmaceutical industry as a tool for monitoring and controlling manufacturing process. Non-contact methods, such as PXRD analysis, near infrared (NIR) spectroscopy and terahertz spectroscopy have been paid attention as important tools for PAT. 6) Chemoinformatics are employed by pre-formulation scientists for the quantitative and qualitative analyses of NIR because they can provide ideal means for extracting quantitative information from complex spectra of mult...

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Section: Quantitative Analysis Of Pharmaceutical Bulk Powders By Pls mentioning

confidence: 99%

Quantification of Pharmaceutical Compounds Based on Powder X-Ray Diffraction with Chemometrics

Otsuka

Itô

Matsumura

et al. 2016

CHEMICAL & PHARMACEUTICAL BULLETIN

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“…A univariate peak area calibration is in principle able to quantify liquid composition even for nonisothermal processes. 43 In order to obtain a calibration model that is applicable over a wide range of process conditions, an extensive calibration set was designed including samples in under-as well as supersaturated regions (see the ESI †). According to our investigations, the signal intensity of the selected band is mainly influenced by the concentration of SLT, and is almost insensitive to temperature.…”

Section: Crystallisationmentioning

confidence: 99%

Crystallisation of a salt hydrate with a complex solid form landscape

et al. 2017

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Different approaches were utilized to assess the thermodynamic stability relationship between four distinct hemihydrates of sitagliptin L-tartrate (SLT). These phases are true polymorphs, having the same chemical composition and molar ratio of water, but different arrangement in the crystal lattice. The general approaches (Burger and Ramberger rules) have only limited applicability, but indicated a monotropic relationship between Phase 1 and Phase 2. The crystallisation and transformation behaviour of the polymorphs was strongly influenced by the solvent composition. As the stability thereof was found to be solvent-dependent, the application of the van't Hoff plot or the solvent-mediated transformation did not unambiguously reveal the relative stability of the forms. Experiments were carried out in an endeavour to determine the most suitable concentration trajectory for cooling crystallisation of the selected candidate and prevent concomitant crystallisation. The application of in situ monitoring techniques, such as FTIR-ATR and FBRM, offered great potential for process optimization and control.

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“…The recent references [13,15] presented rapid PLS-based calibration methods based on the USZ spectra for real-time measurement of the ammonium sulphate and urea crystallization processes, respectively. By comparison, only a few references [16][17][18][19] suggested that the metastable zone (MSZ) spectra should be taken into account for model calibration because the crystallization process is mainly operated in MSZ. It was proposed [16,17] to combine the USZ spectra with the MSZ spectra for calibration to improve prediction accuracy on the solution concentration of potassium dihydrogen phosphate (KDP) and LGA during crystallization, therefore reducing the averaged prediction error to 0.37 g/L solvent for LGA solution.…”

Section: Introductionmentioning

confidence: 99%

“…It was proposed [16,17] to combine the USZ spectra with the MSZ spectra for calibration to improve prediction accuracy on the solution concentration of potassium dihydrogen phosphate (KDP) and LGA during crystallization, therefore reducing the averaged prediction error to 0.37 g/L solvent for LGA solution. Cornel et al [18] used the collected USZ and MSZ spectra together to build a calibration model in terms of the PCR and PLSR algorithms for LGA solution, indicating smaller root mean square error of cross validation (RMSECV) by using PLSR, i.e. 0.186 g/kg solvent.…”

Section: Introductionmentioning

confidence: 99%

Comparative study on ATR-FTIR calibration models for monitoring solution concentration in cooling crystallization

Zhang

Liu

Wang

et al. 2017

Journal of Crystal Growth

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Abstract:In this paper calibration model building based on using an ATR-FTIR spectroscopy is investigated for in-situ measurement of the solution concentration during a cooling crystallization process. The cooling crystallization of L-glutamic Acid (LGA) as a case is studied here. It was found that using the metastable zone (MSZ) data for model calibration can contribute to the prediction accuracy, compared to the usage of undersaturated zone (USZ) spectra as traditionally practiced which may lead to undesired bias for prediction of the MSZ concentration. Calibration experiments were made for LGA solution under different concentrations. Four candidate calibration models were established using different zone data for comparison, based on a multivariate partial least-squares (PLS) regression algorithm for the collected spectra together with the corresponding temperature values. Experiments under varied concentrations and operational changes of temperature were conducted. The results indicate that using MSZ spectra for model calibration can give more accurate prediction of the solution concentration during the crystallization process. The primary reason was clarified as spectral nonlinearity for measurement between USZ and MSZ. In addition, an LGA cooling crystallization experiment was performed to verify the sensitivity of these calibration models for monitoring the crystal growth process.

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Quantitative Application of in Situ ATR-FTIR and Raman Spectroscopy in Crystallization Processes

Cited by 132 publications

References 41 publications

Quantification of Pharmaceutical Compounds Based on Powder X-Ray Diffraction with Chemometrics

Quantification of Pharmaceutical Compounds Based on Powder X-Ray Diffraction with Chemometrics

Crystallisation of a salt hydrate with a complex solid form landscape

Comparative study on ATR-FTIR calibration models for monitoring solution concentration in cooling crystallization

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