Selected papers from the latest issue:
Identification of Genistein and Biochanin A by THz (far-infrared) Vibrational Spectra
21 December 2011, 01:50:06
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 20 December 2011
Yuping Yang, S. Sree Harsha, Alisha J. Shutler, Daniel R. Grischkowsky
The temperature dependent vibrational spectra of Genestein and Biochanin A, major components in Mongolian medicinesAgi, in the range of 0.5-4.5 THz (16.7-150 cm) are presented for the first time. Over the temperature range from 295 to 77 K, 12 highly resolved spectral features for the Genestein and 13 features for Biochanin A were measured by THz-TDS and display strong linewidth narrowing and frequency blue-shift with cooling. Such narrow-line THz fingerprint spectra provide a rapid, nondestructive and reliable method for the identification of these Chinese traditional medicines.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 20 December 2011
Yuping Yang, S. Sree Harsha, Alisha J. Shutler, Daniel R. Grischkowsky
The temperature dependent vibrational spectra of Genestein and Biochanin A, major components in Mongolian medicinesAgi, in the range of 0.5-4.5 THz (16.7-150 cm) are presented for the first time. Over the temperature range from 295 to 77 K, 12 highly resolved spectral features for the Genestein and 13 features for Biochanin A were measured by THz-TDS and display strong linewidth narrowing and frequency blue-shift with cooling. Such narrow-line THz fingerprint spectra provide a rapid, nondestructive and reliable method for the identification of these Chinese traditional medicines.
Highlights
► For the first time the THz-TDS technique has been used to measure the far-infrared spectra of the important anti-carcinogenic compounds Genistein and Biochanin A. ► Over the temperature range from 295 to 77 K, 12 highly resolved spectral features for Genestein and 13 features for Biochanin A were observed over the spectral range from 0.5 to 4.5 THz (from 16.5 to 150 cm). ► With such narrow-line THz fingerprint spectra, it now becomes possible to achieve a full understanding of these molecules and to provide a rapid, nondestructive and reliable method for identification of these Chinese traditional medicines.Development of chromatographic methods for the determination of genotoxic impurities in cloperastine fendizoate
21 December 2011, 01:50:06
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 19 December 2011
Antonia García, Francisco J Rupérez, Florencia Ceppa, Federica Pellati, Coral Barbas
The classification of an impurity of a drug substance as genotoxic means that the “Threshold of Toxicological Concern” (TTC) value of 1.5 μg/day intake, considered to be associated with an acceptable risk, should be the admissible limit in the raw material and that leads to new analytical challenges. In this study, reliable chromatographic methods were developed and applied aslimit tests for the control of three genotoxic impurities (GTIs) in cloperastine fendizoate, drug widely used as an antitussive active pharmaceutical ingredient (API). In particular, GC-MS was applied to the determination of one alkyl halide (2-chloroethanol, 2-CE), while HPLC-DAD was selected for the analysis of two sulfonate esters (methylp-toluenesulfonate, MPTS, and 2-chloroethylp-toluenesulfonate, CEPTS).Regarding GC-MS, strong anion-exchange (SAX)-SPE was applied to remove fendizoate from the sample solutions, due its low volatility and its high amount in the raw material. The GC-MS analysis was performed on a Factor Four VF-23ms capillary column (30 m x 0.25 mm I.D., film thickness 0.25 μm, Varian). Single ion-monitoring (SIM) detection mode was set atm/z80.In the case of HPLC-DAD, a suitable optimization of the chromatographic conditions was carried out in order to obtain a good separation of the impurity peaks from the drug substance peaks. The optimized method utilizes a SymmetryShield RP8column (250 × 4.6 mm, 5 μm, Waters) kept at 50 °C, with phosphate buffer (pH 3.0; 10 mM)-methanol (containing 10% ACN) (45:55, v/v) as the mobile phase, at the flow-rate of 1.7 mL/min and UV detection at 227 nm. The required sensitivity level was achieved by injecting 80 μL of sample solution, purified from fendizoate by SAX-SPE, followed by a 1:1 (v/v) dilution of the SPE eluate with water.For both GC-MS and HPLC-DAD, the method validation was performed in relation to specificity and limit of detection (LOD), as required by ICH guidelines in relation to limit assays. The developed methods were successfully applied for the determination of GTIs in five different batches of cloperastine fendizoate. In all the analyzed batches, the three target GTIs were below the concentration limit.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 19 December 2011
Antonia García, Francisco J Rupérez, Florencia Ceppa, Federica Pellati, Coral Barbas
The classification of an impurity of a drug substance as genotoxic means that the “Threshold of Toxicological Concern” (TTC) value of 1.5 μg/day intake, considered to be associated with an acceptable risk, should be the admissible limit in the raw material and that leads to new analytical challenges. In this study, reliable chromatographic methods were developed and applied aslimit tests for the control of three genotoxic impurities (GTIs) in cloperastine fendizoate, drug widely used as an antitussive active pharmaceutical ingredient (API). In particular, GC-MS was applied to the determination of one alkyl halide (2-chloroethanol, 2-CE), while HPLC-DAD was selected for the analysis of two sulfonate esters (methylp-toluenesulfonate, MPTS, and 2-chloroethylp-toluenesulfonate, CEPTS).Regarding GC-MS, strong anion-exchange (SAX)-SPE was applied to remove fendizoate from the sample solutions, due its low volatility and its high amount in the raw material. The GC-MS analysis was performed on a Factor Four VF-23ms capillary column (30 m x 0.25 mm I.D., film thickness 0.25 μm, Varian). Single ion-monitoring (SIM) detection mode was set atm/z80.In the case of HPLC-DAD, a suitable optimization of the chromatographic conditions was carried out in order to obtain a good separation of the impurity peaks from the drug substance peaks. The optimized method utilizes a SymmetryShield RP8column (250 × 4.6 mm, 5 μm, Waters) kept at 50 °C, with phosphate buffer (pH 3.0; 10 mM)-methanol (containing 10% ACN) (45:55, v/v) as the mobile phase, at the flow-rate of 1.7 mL/min and UV detection at 227 nm. The required sensitivity level was achieved by injecting 80 μL of sample solution, purified from fendizoate by SAX-SPE, followed by a 1:1 (v/v) dilution of the SPE eluate with water.For both GC-MS and HPLC-DAD, the method validation was performed in relation to specificity and limit of detection (LOD), as required by ICH guidelines in relation to limit assays. The developed methods were successfully applied for the determination of GTIs in five different batches of cloperastine fendizoate. In all the analyzed batches, the three target GTIs were below the concentration limit.
Highlights
► Determination of genotoxic impurities with different physico-chemical properties in cloperastine phendizoate at ppb level.A method for identifying the origin of chondroitin sulfate with near infrared spectroscopy
20 December 2011, 01:23:35
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 19 December 2011
Hengchang Zang, Lian li, Fengshan Wang, Qiong Yi, Qin Dong, ...
The object of this study was to explore the feasibility of support vector machine (SVM) to identify the origin of chondroitin sulfate (CS) by near infrared spectroscopy. 96 batches CS from three different origins were collected in this research, 66 batches of which were chosen for training set by Kennard–Stone (KS) method and the rest were used for testing. Through the comparison of pretreatment methods of standard normal variate transformation (SNV), multiplicative scatter correction (MSC), Savitzky-Golay (SG) smoothing and derivative with SG smoothing, a SVM discrimination model was constructed, of which the prediction result is 100% accurate with the pretreatment of first derivative and SG smoothing with 15 points. The result indicated that it had great potential using SVM to identify the origin of CS.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 19 December 2011
Hengchang Zang, Lian li, Fengshan Wang, Qiong Yi, Qin Dong, ...
The object of this study was to explore the feasibility of support vector machine (SVM) to identify the origin of chondroitin sulfate (CS) by near infrared spectroscopy. 96 batches CS from three different origins were collected in this research, 66 batches of which were chosen for training set by Kennard–Stone (KS) method and the rest were used for testing. Through the comparison of pretreatment methods of standard normal variate transformation (SNV), multiplicative scatter correction (MSC), Savitzky-Golay (SG) smoothing and derivative with SG smoothing, a SVM discrimination model was constructed, of which the prediction result is 100% accurate with the pretreatment of first derivative and SG smoothing with 15 points. The result indicated that it had great potential using SVM to identify the origin of CS.
No comments:
Post a Comment