Wataru Momose - Academia.edu (original) (raw)
Papers by Wataru Momose
Journal of pharmaceutical and biomedical analysis, Jan 5, 2016
Film-coated tablets (FCTs) are a popular solid dosage form in pharmaceutical industry. Manufactur... more Film-coated tablets (FCTs) are a popular solid dosage form in pharmaceutical industry. Manufacturing conditions during the film-coating process affect the properties of the film layer, which might result in critical quality problems. Here, we analyzed the properties of the film layer using a non-destructive approach with terahertz pulsed imaging (TPI). Hydrophilic tablets that become distended upon water absorption were used as core tablets and coated with film under different manufacturing conditions. TPI-derived parameters such as film thickness (FT), film surface reflectance (FSR), and interface density difference (IDD) between the film layer and core tablet were affected by manufacturing conditions and influenced critical quality attributes of FCTs. Relative standard deviation of FSR within tablets correlated well with surface roughness. Tensile strength could be predicted in a non-destructive manner using the multivariate regression equation to estimate the core tablet density ...
Journal of Pharmaceutical Innovation, 2014
ABSTRACT An approach for the efficient development of near-infrared (NIR) methods for blend analy... more ABSTRACT An approach for the efficient development of near-infrared (NIR) methods for blend analysis using simulated real blending conditions is described. Spectra used to calculate a model were collected from small volume pharmaceutical blends in a die subject to well-controlled forces. Blend end-point detection by NIR spectroscopy is widely used. Strategic deployment of analytical technology is critical to companies seeking to utilize quality by design (QbD) and process analytical technology (PAT) concepts. However, pilot and commercial scale experiments using near-infrared spectroscopy (NIRS) are often limited due to resources. Specifically, limitations to the quantity of active pharmaceutical ingredients (APIs) available during development stage can dissuade early PAT method development. Such experiments are often necessary due to substantial differences between NIR data collected from small-scale (laboratory) blend systems and larger scale equipment. In the present work, data collected from small samples of pharmaceutical powders placed in an Instron testing station under carefully controlled forces matched conditions of the same powders in a blender. Use of this strategy for development of NIR-based blend end-point methods requires minimal quantities of pharmaceutical powders. Principal component analysis (PCA), two-dimensional (2D) correlation spectroscopy analysis, and Hotelling’s T2 ellipse results demonstrated that NIR spectra obtained in the small die matched NIR spectra in a blender when forces to the die were carefully applied. This strategy has the potential to significantly reduce the cost of development of NIR methods for blending.
Results in Pharma Sciences, 2012
Here, we describe a nondestructive approach using terahertz wave to detect crack initiation in a ... more Here, we describe a nondestructive approach using terahertz wave to detect crack initiation in a filmcoated layer on a drug tablet. During scale-up and scale-down of the film coating process, differences in film density and gaps between the film-coated layer and the uncoated tablet were generated due to differences in film coating process parameters, such as the tablet-filling rate in the coating machine, spray pressure, and gas-liquid ratio etc. Tablets using the PEO/PEG formulation were employed as uncoated tablets. We found that heat and humidity caused tablets to swell, thereby breaking the filmcoated layer. Using our novel approach with terahertz wave nondestructively detect film surface density (FSD) and interface density differences (IDDs) between the film-coated layer and an uncoated tablet. We also found that a reduced FSD and IDD between the film-coated layer and uncoated tablet increased the risk of crack initiation in the film-coated layer, thereby enabling us to nondestructively predict initiation of cracks in the film-coated layer. Using this method, crack initiation can be nondestructively assessed in swelling tablets after the film coating process without conducting accelerated stability tests, and film coating process parameters during scale-up and scale-down studies can be appropriately established.
ABSTRACT Here, we describe an approach for creation of matched near-infrared absorption spectra o... more ABSTRACT Here, we describe an approach for creation of matched near-infrared absorption spectra of pharmaceutical powders in a blender by using a small amount of pharmaceutical blends in a die and well-controlled application of force. Recently, pharmaceutical development has followed quality by design (QbD) concepts. Pharmaceutical companies are increasingly using near-infrared spectroscopy (NIRS) as a quality monitoring tool for their products from development stages to commercial productions. Such applications are integral for process control strategies and real time release testing (RTRt). NIRS is a mature process analytical technology (PAT) tool. It has been widely applied for blend-endpoint monitoring. However, the resources required to conduct development experiments at pilot and commercial scale are often prohibitive because of limited supply and costs of active pharmaceutical ingredients (APIs). Such trials are frequently critical because the differences of the process scale have a large impact on NIR spectra. These differences in NIR spectra prevent the simple transfer of a model for predicting concentration from small scale development equipment to pilot or commercial scale. Transfer from the lab scale to larger scale is based on simulating the effect of scale in the laboratory environment using small amounts of material. Careful application of force to pharmaceutical blends in a small die matched conditions of pharmaceutical blends at different scales. A small amount of material in a 5cm die was only used for these blend simulation studies. The impact of this work is that fully transferable methods are developed using small quantities of pharmaceutical blends ( << 1 kg). Principal component analysis (PCA), two-dimensional (2D) correlation spectroscopy analysis and Hotteling’s T2 ellipse results demonstrated that NIR spectra obtained in the experimental apparatus matched NIR spectra in a blender. This approach has the potential to dramatically reduce the material costs used for NIRS research of blending process.
ICH Q8,Q9,Q10,Q11各個別の導入/活用手法を各社実例に基づいて解説 ICH Qトリオに対してどのように取り組むべきか？Q11はどう影響するのか？ ICH Q11の導入手法と活用方法... more ICH Q8,Q9,Q10,Q11各個別の導入/活用手法を各社実例に基づいて解説 ICH Qトリオに対してどのように取り組むべきか？Q11はどう影響するのか？ ICH Q11の導入手法と活用方法を解説！ グローバルスタンダードに適応するための品質管理への理解と現場への導入方法
Powder Technology, 2011
Here, we describe a combination approach using Two Calibration-Free Methods with reflectance near... more Here, we describe a combination approach using Two Calibration-Free Methods with reflectance nearinfrared (TCFM-NIR), which involves detecting end-points for active pharmaceutical ingredients (APIs) blending by simultaneously monitoring specific NIR peak intensity of APIs and calculating moving block standard deviation (MBSD). After determining the specific NIR peak range of nicaldipine hydrochloride, conditions for TCFM-NIR were established by monitoring the differential intensity of the second peak (1136 nm) while MBSD was calculated from the NIR peak intensity between 1100 and 1150 nm. In comparison with the validated reference method of UV-VIS spectroscopy, which is particularly destructive, TCFM-NIR was found to be useful in detecting end-points for blending of nicaldipine hydrochloride. TCFM-NIR monitors two important factors for estimation of blend uniformity: API concentration, using specific NIR peak intensity for APIs, and blend homogeneity, using MBSD. Also, the conditions of TCFM-NIR were confirmed to be adequate by using Partial Least Square (PLS). Further, simultaneously monitoring these two blend uniformity factors is more useful in preventing estimation errors for nondestructive monitoring of blend homogeneity than monitoring only one factor, as with NIR spectroscopy.
JOURNAL OF CHEMICAL ENGINEERING OF JAPAN, 2004
ABSTRACT Partially carbonized polyimide (CPI) membranes were prepared on a porous alumina support... more ABSTRACT Partially carbonized polyimide (CPI) membranes were prepared on a porous alumina support from carbonization of polyimide membranes at 460-500degreesC. The permeance of O-2 through the CPI membrane increased with the increasing carbonization temperature, although the separation factors (O-2/(N)2) reduced from 11 to 4. The highly permeable CPI membranes carbonized at 500degreesC were silylated with 1,1,1,3,3,3-hexamethyl disilazane (HMDS) at 90degreesC, 150degreesC and 180degreesC before or after carbonization to solve an adverse humidity effect on gas permeation. The molar ratios of C/Si in the cross section of the silylated CPI membranes were analyzed by SEM-EDX measurements. The separation of dry air through the nonsilylated and silylated CPI membranes was performed before and after a steam treatment. Continuous air permeation tests under saturated steam were also performed with prolonged time. The CPI membranes silylated at 180degreesC had deposition of organosilicate on the outer surface of polyamide layer, resulting in the reduction of the O-2 flux. On the other hand, the flux of O-2 and the separation factor for the CPI membrane silylated at 150degreesC before carbonization did not reduce drastically under saturated steam. The results of chemical composition analysis for polyimide and carbonized polyimide suggests that water-resistant CPI membranes with high O-2 permeation flux were synthesized by taking advantage of reactive carboxyl groups in the membrane before carbonization.
JOURNAL OF CHEMICAL ENGINEERING OF JAPAN, 2003
ABSTRACT Partially carbonized polyimide (CPI) membranes were prepared from a solution of 30 wt% p... more ABSTRACT Partially carbonized polyimide (CPI) membranes were prepared from a solution of 30 wt% polyamic acid in N, N-dimethylacetamide. The polymer membranes formed on an alumina support were thermally treated, involving imidization in air at 180°C and carbonization in N2 at relatively low temperature (400–500°C). The cross-sectional views of the supported CPI membranes show that the membranes consist of a top layer (thickness, 10 μm) on the support and a CPI/alumina thin layer in the support. The CPI membranes carbonized at 500°C showed high permeability for O2 of 1000–30000 barrer and permselectivity for O2/N2 of 3–6. The permeability of the CPI membranes was much higher than that of the reported polymer membranes and the carbon membranes. The pores formed under carbonization at 500°C and 400°C were effective for separating O2/N2 and CO2/CH4 mixtures, respectively. TG analysis indicated that the carbonization proceeds even at a constant temperature of 500°C. The successive generation of flexible pores before the formation of graphite structure with rigid pores seems to contribute to the higher permeability of the CPI membranes.
Advanced Powder Technology, 2014
ABSTRACT For process control of fluidized bed granulation process, we investigated proportional (... more ABSTRACT For process control of fluidized bed granulation process, we investigated proportional (P) moisture content control via adjustment of inlet air temperature in proportion to the difference between measured and target moisture content of granules. Here, we first validated P moisture content control by comparison with bed temperature control. We then confirmed that P moisture content control is effective in maintaining the moisture content, and in minimizing the variance of the particle size of granules following granulation. Furthermore, we observed that when the target temperature was higher than the measured value of inlet air temperature the P moisture content control response was accelerated. In contrast, when the target temperature was less than the measured value of inlet air temperature (<50 °C) the response was delayed. In summary, P moisture content control has good scalability and can be introduced without changing granulation conditions in the development of orally administered pharmaceutical products.
ABSTRACT Critical quality attributes of film coatings, such as coating layer thickness and unifor... more ABSTRACT Critical quality attributes of film coatings, such as coating layer thickness and uniformity, are often determined via indirect measurements. Traditional weight-gain calculations are used to determine the endpoint of coating processes. Such calculations do not offer sufficient information about the coating integrity, which is usually a major concern in pharmaceutical production. Other technologies such as imaging analysis can be used to investigate the film thickness and integrity, however are destructive and require laborious work for samples preparation. The purposes of this work were: (1) to investigate the capability of terahertz spectroscopy to characterize, in a non-destructive manner, the statistical coating thickness distribution of coated multiparticulate dosage forms; (2) to be used as an advanced reference method for developing an in-line NIR quantitative model for the film thickness process control. Non-pareil beads were used as the coating substrates, Eudragit NE 30 D aqueous dispersion was used as the main sustained release coating material. The coating processes were performed in a laboratory scale top-spray fluidized bed processor, important process parameters were carefully controlled to achieve good coating conditions. Near-Infrared spectrometer was used to monitor the coating processes, coated samples were collected at each pre-determined time point. Imaging analysis and terahertz spectroscopy were both used in this work as reference methods. Calibration models were generated for film coating thickness quantification using partial-least squares (PLS) regression. Film coating thickness and uniformity in the useful coating range can be determined by Terahertz spectroscopy. In-line NIR quantitative model can be developed using terahertz spectroscopy as reference method, and the model showed good predicting power with acceptable prediction error. Terahertz spectroscopy can be used for the development of real time monitoring process control tools in coating technologies.
Journal of pharmaceutical and biomedical analysis, Jan 5, 2016
Film-coated tablets (FCTs) are a popular solid dosage form in pharmaceutical industry. Manufactur... more Film-coated tablets (FCTs) are a popular solid dosage form in pharmaceutical industry. Manufacturing conditions during the film-coating process affect the properties of the film layer, which might result in critical quality problems. Here, we analyzed the properties of the film layer using a non-destructive approach with terahertz pulsed imaging (TPI). Hydrophilic tablets that become distended upon water absorption were used as core tablets and coated with film under different manufacturing conditions. TPI-derived parameters such as film thickness (FT), film surface reflectance (FSR), and interface density difference (IDD) between the film layer and core tablet were affected by manufacturing conditions and influenced critical quality attributes of FCTs. Relative standard deviation of FSR within tablets correlated well with surface roughness. Tensile strength could be predicted in a non-destructive manner using the multivariate regression equation to estimate the core tablet density ...
Journal of Pharmaceutical Innovation, 2014
ABSTRACT An approach for the efficient development of near-infrared (NIR) methods for blend analy... more ABSTRACT An approach for the efficient development of near-infrared (NIR) methods for blend analysis using simulated real blending conditions is described. Spectra used to calculate a model were collected from small volume pharmaceutical blends in a die subject to well-controlled forces. Blend end-point detection by NIR spectroscopy is widely used. Strategic deployment of analytical technology is critical to companies seeking to utilize quality by design (QbD) and process analytical technology (PAT) concepts. However, pilot and commercial scale experiments using near-infrared spectroscopy (NIRS) are often limited due to resources. Specifically, limitations to the quantity of active pharmaceutical ingredients (APIs) available during development stage can dissuade early PAT method development. Such experiments are often necessary due to substantial differences between NIR data collected from small-scale (laboratory) blend systems and larger scale equipment. In the present work, data collected from small samples of pharmaceutical powders placed in an Instron testing station under carefully controlled forces matched conditions of the same powders in a blender. Use of this strategy for development of NIR-based blend end-point methods requires minimal quantities of pharmaceutical powders. Principal component analysis (PCA), two-dimensional (2D) correlation spectroscopy analysis, and Hotelling’s T2 ellipse results demonstrated that NIR spectra obtained in the small die matched NIR spectra in a blender when forces to the die were carefully applied. This strategy has the potential to significantly reduce the cost of development of NIR methods for blending.
Results in Pharma Sciences, 2012
Here, we describe a nondestructive approach using terahertz wave to detect crack initiation in a ... more Here, we describe a nondestructive approach using terahertz wave to detect crack initiation in a filmcoated layer on a drug tablet. During scale-up and scale-down of the film coating process, differences in film density and gaps between the film-coated layer and the uncoated tablet were generated due to differences in film coating process parameters, such as the tablet-filling rate in the coating machine, spray pressure, and gas-liquid ratio etc. Tablets using the PEO/PEG formulation were employed as uncoated tablets. We found that heat and humidity caused tablets to swell, thereby breaking the filmcoated layer. Using our novel approach with terahertz wave nondestructively detect film surface density (FSD) and interface density differences (IDDs) between the film-coated layer and an uncoated tablet. We also found that a reduced FSD and IDD between the film-coated layer and uncoated tablet increased the risk of crack initiation in the film-coated layer, thereby enabling us to nondestructively predict initiation of cracks in the film-coated layer. Using this method, crack initiation can be nondestructively assessed in swelling tablets after the film coating process without conducting accelerated stability tests, and film coating process parameters during scale-up and scale-down studies can be appropriately established.
ABSTRACT Here, we describe an approach for creation of matched near-infrared absorption spectra o... more ABSTRACT Here, we describe an approach for creation of matched near-infrared absorption spectra of pharmaceutical powders in a blender by using a small amount of pharmaceutical blends in a die and well-controlled application of force. Recently, pharmaceutical development has followed quality by design (QbD) concepts. Pharmaceutical companies are increasingly using near-infrared spectroscopy (NIRS) as a quality monitoring tool for their products from development stages to commercial productions. Such applications are integral for process control strategies and real time release testing (RTRt). NIRS is a mature process analytical technology (PAT) tool. It has been widely applied for blend-endpoint monitoring. However, the resources required to conduct development experiments at pilot and commercial scale are often prohibitive because of limited supply and costs of active pharmaceutical ingredients (APIs). Such trials are frequently critical because the differences of the process scale have a large impact on NIR spectra. These differences in NIR spectra prevent the simple transfer of a model for predicting concentration from small scale development equipment to pilot or commercial scale. Transfer from the lab scale to larger scale is based on simulating the effect of scale in the laboratory environment using small amounts of material. Careful application of force to pharmaceutical blends in a small die matched conditions of pharmaceutical blends at different scales. A small amount of material in a 5cm die was only used for these blend simulation studies. The impact of this work is that fully transferable methods are developed using small quantities of pharmaceutical blends ( << 1 kg). Principal component analysis (PCA), two-dimensional (2D) correlation spectroscopy analysis and Hotteling’s T2 ellipse results demonstrated that NIR spectra obtained in the experimental apparatus matched NIR spectra in a blender. This approach has the potential to dramatically reduce the material costs used for NIRS research of blending process.
ICH Q8,Q9,Q10,Q11各個別の導入/活用手法を各社実例に基づいて解説 ICH Qトリオに対してどのように取り組むべきか？Q11はどう影響するのか？ ICH Q11の導入手法と活用方法... more ICH Q8,Q9,Q10,Q11各個別の導入/活用手法を各社実例に基づいて解説 ICH Qトリオに対してどのように取り組むべきか？Q11はどう影響するのか？ ICH Q11の導入手法と活用方法を解説！ グローバルスタンダードに適応するための品質管理への理解と現場への導入方法
Powder Technology, 2011
Here, we describe a combination approach using Two Calibration-Free Methods with reflectance near... more Here, we describe a combination approach using Two Calibration-Free Methods with reflectance nearinfrared (TCFM-NIR), which involves detecting end-points for active pharmaceutical ingredients (APIs) blending by simultaneously monitoring specific NIR peak intensity of APIs and calculating moving block standard deviation (MBSD). After determining the specific NIR peak range of nicaldipine hydrochloride, conditions for TCFM-NIR were established by monitoring the differential intensity of the second peak (1136 nm) while MBSD was calculated from the NIR peak intensity between 1100 and 1150 nm. In comparison with the validated reference method of UV-VIS spectroscopy, which is particularly destructive, TCFM-NIR was found to be useful in detecting end-points for blending of nicaldipine hydrochloride. TCFM-NIR monitors two important factors for estimation of blend uniformity: API concentration, using specific NIR peak intensity for APIs, and blend homogeneity, using MBSD. Also, the conditions of TCFM-NIR were confirmed to be adequate by using Partial Least Square (PLS). Further, simultaneously monitoring these two blend uniformity factors is more useful in preventing estimation errors for nondestructive monitoring of blend homogeneity than monitoring only one factor, as with NIR spectroscopy.
JOURNAL OF CHEMICAL ENGINEERING OF JAPAN, 2004
ABSTRACT Partially carbonized polyimide (CPI) membranes were prepared on a porous alumina support... more ABSTRACT Partially carbonized polyimide (CPI) membranes were prepared on a porous alumina support from carbonization of polyimide membranes at 460-500degreesC. The permeance of O-2 through the CPI membrane increased with the increasing carbonization temperature, although the separation factors (O-2/(N)2) reduced from 11 to 4. The highly permeable CPI membranes carbonized at 500degreesC were silylated with 1,1,1,3,3,3-hexamethyl disilazane (HMDS) at 90degreesC, 150degreesC and 180degreesC before or after carbonization to solve an adverse humidity effect on gas permeation. The molar ratios of C/Si in the cross section of the silylated CPI membranes were analyzed by SEM-EDX measurements. The separation of dry air through the nonsilylated and silylated CPI membranes was performed before and after a steam treatment. Continuous air permeation tests under saturated steam were also performed with prolonged time. The CPI membranes silylated at 180degreesC had deposition of organosilicate on the outer surface of polyamide layer, resulting in the reduction of the O-2 flux. On the other hand, the flux of O-2 and the separation factor for the CPI membrane silylated at 150degreesC before carbonization did not reduce drastically under saturated steam. The results of chemical composition analysis for polyimide and carbonized polyimide suggests that water-resistant CPI membranes with high O-2 permeation flux were synthesized by taking advantage of reactive carboxyl groups in the membrane before carbonization.
JOURNAL OF CHEMICAL ENGINEERING OF JAPAN, 2003
ABSTRACT Partially carbonized polyimide (CPI) membranes were prepared from a solution of 30 wt% p... more ABSTRACT Partially carbonized polyimide (CPI) membranes were prepared from a solution of 30 wt% polyamic acid in N, N-dimethylacetamide. The polymer membranes formed on an alumina support were thermally treated, involving imidization in air at 180°C and carbonization in N2 at relatively low temperature (400–500°C). The cross-sectional views of the supported CPI membranes show that the membranes consist of a top layer (thickness, 10 μm) on the support and a CPI/alumina thin layer in the support. The CPI membranes carbonized at 500°C showed high permeability for O2 of 1000–30000 barrer and permselectivity for O2/N2 of 3–6. The permeability of the CPI membranes was much higher than that of the reported polymer membranes and the carbon membranes. The pores formed under carbonization at 500°C and 400°C were effective for separating O2/N2 and CO2/CH4 mixtures, respectively. TG analysis indicated that the carbonization proceeds even at a constant temperature of 500°C. The successive generation of flexible pores before the formation of graphite structure with rigid pores seems to contribute to the higher permeability of the CPI membranes.
Advanced Powder Technology, 2014
ABSTRACT For process control of fluidized bed granulation process, we investigated proportional (... more ABSTRACT For process control of fluidized bed granulation process, we investigated proportional (P) moisture content control via adjustment of inlet air temperature in proportion to the difference between measured and target moisture content of granules. Here, we first validated P moisture content control by comparison with bed temperature control. We then confirmed that P moisture content control is effective in maintaining the moisture content, and in minimizing the variance of the particle size of granules following granulation. Furthermore, we observed that when the target temperature was higher than the measured value of inlet air temperature the P moisture content control response was accelerated. In contrast, when the target temperature was less than the measured value of inlet air temperature (<50 °C) the response was delayed. In summary, P moisture content control has good scalability and can be introduced without changing granulation conditions in the development of orally administered pharmaceutical products.
ABSTRACT Critical quality attributes of film coatings, such as coating layer thickness and unifor... more ABSTRACT Critical quality attributes of film coatings, such as coating layer thickness and uniformity, are often determined via indirect measurements. Traditional weight-gain calculations are used to determine the endpoint of coating processes. Such calculations do not offer sufficient information about the coating integrity, which is usually a major concern in pharmaceutical production. Other technologies such as imaging analysis can be used to investigate the film thickness and integrity, however are destructive and require laborious work for samples preparation. The purposes of this work were: (1) to investigate the capability of terahertz spectroscopy to characterize, in a non-destructive manner, the statistical coating thickness distribution of coated multiparticulate dosage forms; (2) to be used as an advanced reference method for developing an in-line NIR quantitative model for the film thickness process control. Non-pareil beads were used as the coating substrates, Eudragit NE 30 D aqueous dispersion was used as the main sustained release coating material. The coating processes were performed in a laboratory scale top-spray fluidized bed processor, important process parameters were carefully controlled to achieve good coating conditions. Near-Infrared spectrometer was used to monitor the coating processes, coated samples were collected at each pre-determined time point. Imaging analysis and terahertz spectroscopy were both used in this work as reference methods. Calibration models were generated for film coating thickness quantification using partial-least squares (PLS) regression. Film coating thickness and uniformity in the useful coating range can be determined by Terahertz spectroscopy. In-line NIR quantitative model can be developed using terahertz spectroscopy as reference method, and the model showed good predicting power with acceptable prediction error. Terahertz spectroscopy can be used for the development of real time monitoring process control tools in coating technologies.