UPLC is an advance technique of liquid chromatography where it takes advantage of innovation in v... more UPLC is an advance technique of liquid chromatography where it takes advantage of innovation in various technologies such as instrumentation and particle size to achieve dramatic increases in resolution, speed and sensitivity of the liquid chromatography. It operates at higher pressure than that used in HPLC and uses fine particles (less than 2.5µm) & mobile phases at high linear velocities. UPLC Technology is now applied throughout the world produce quality data with reproducible and robust methods as compared to the conventional HPLC. UPLC can be hyphenated with other techniques such as Mass spectrometer (MS), Ion chromatograph (IC), Nuclear magnetic resonance spectrometer (NMR) and Infrared spectrometer (IR) etc. This technique provides unique end-to-end solutions for all industries and has found application in various fields such as pharmaceutical, food, environmental, forensic, toxicology and pesticide.
Nitrosamine impurities are known to be mutagenic and carcinogenic, very small exposure of these i... more Nitrosamine impurities are known to be mutagenic and carcinogenic, very small exposure of these impurities can lead to cancer. These impurities may be formed and get incorporated into drug substance or drug product through reagent, catalyst, solvent or raw materials used in the process of manufacturing. The various regulatory authority has published the press release or notice regarding the control of these impurities with the interim limit. Nitrosamine impurities can be avoided by taking precaution in the manufacturing of drug substance and drug products. Validated analytical methods are to be used to identify and quantify these impurities hence it needs highly sensitive instrument which can detect these impurities to the trace level at given interim limit. Liquid chromatography or Gas chromatography, along with mass detector is majorly used for their determination.
Impurities are unwanted chemical substances present in the Pharmaceutical drug products and drug ... more Impurities are unwanted chemical substances present in the Pharmaceutical drug products and drug substances with no therapeutic benefits or some time potential to harm patient safety if present above a certain limit. The basic need in manufacturing of safe and good quality of drug substances and drug product, control of impurities is very necessary for the pharmaceutical industry. Several regulatory agencies have formulated guidelines for the control of these impurities. The present review article describes the impurities, origin of impurities, classification of impurities, control limit of impurities, guidelines for their control, isolation of impurities and its characterization using various analytical techniques.
Environmental pollution is majorly caused by the chemical and pharmaceutical industries which hav... more Environmental pollution is majorly caused by the chemical and pharmaceutical industries which have increased multifold time in the last several decades. It is the responsibility of science to design the process which will generate the less hazardous chemicals and much environmentally friendly waste. Ionic liquid finds a source of hope in reducing the organic solvent waste in coming years. These Ionic liquids may replace the organic solvents which are hazardous, toxic and non-environmentally friendly used in the synthesis of chemical compounds. This review article describes the Introduction to Ionic liquids, their types and classification, the advantages of their use in replacement of organic solvent in the synthesis of chemicals compounds and drug substances.
A rapid, sensitive and highly selective High performance liquid chromatography (HPLC) method was ... more A rapid, sensitive and highly selective High performance liquid chromatography (HPLC) method was developed and validated for the determination of trace level Genotoxic Melamine impurity, as required by USFDA and that may be present in Allopurinol. HPLC column used was Cosmosil C18 (250 x 4.6 mm, 5µm). The isocratic elution modewas selected where the mobile phaseconsists of 1.25 g/l Sodium dihydrogen phosphate solution. The flow rate was set to1.0 mL/minand run time of 30 minutes. UV detector with wavelength 208 nm was used for theanalysis. The column oven temperature was kept at 25°C. The developed method was validated according to ICH guideline and found to be linear in the range of 5.20 ppm to 52.05 ppm with a correlation coefficient 0.9997. Limit of detection and limit of quantitation was found to be 1.21 ppm and 3.68 ppm respectively. Recovery for this impurity was found between 93.37% and 107.59%.A method was found to be specific, selective, precise, and robust. The developed method can successfully be applied for the determination of Genotoxic Melamine impurity in Allopurinol.
A simple, precise, linear, accurate and robust spectrophotometric method was developed for the es... more A simple, precise, linear, accurate and robust spectrophotometric method was developed for the estimation of palladium content in Rasagiline Mesylate. The proposed method is based on complex formation of palladium with α-nitroso-β-napthol in alkaline medium and extraction with toluene and estimation. The spectrum shows maximum absorption at 425 nm. The method is validated as per on International council for harmonization (ICH) guidelines. The absorbance-concentration plot is linear over the concentration range of 3.08 to15.38 ppm with limit of detection (LOD) of 0.06 ppm and limit of quantification (LOQ) of 0.17 ppm. The recovery of Palladium in Rasagiline Mesylate obtained was between 95 to 105 %. The proposed method can be applied for the determination of palladium content in Rasagiline Mesylate. Original Research Article Hussain et al.; BJPR, 15(4): 1-7, 2017; Article no.BJPR.32254 2
A rapid, sensitive and selective High performance liquid chromatography (HPLC) method was develop... more A rapid, sensitive and selective High performance liquid chromatography (HPLC) method was developed and validated for the trace analysis of N-(2-Chloroallyl)-1-(R)-aminoindan, a potential genotoxic impurity in Rasagiline mesylate drug substances. HPLC column used was Sunfire C18 (250 mm x 4.6 mm, 5 μm). The gradient elution mode was selected where mobile phase-A consist of Buffer (40Mm Ammonium dihydrogen phosphate solution adjusted to pH 7.0 with orthophosphoric acid) and mobile phase-B in 60:40 ratio, whereas mobile phase B consist of solvent Acetonitrile and Methanol in the ratio 70:30. The flow rate was set to 1.5 mL/min and run time of 35 minutes. UV detector with wavelength 210 nm was used for the analysis. Column oven temperature was kept 40°C. The developed method was validated according ICH guideline and found to be linear in the range of 0.51 ppm to 1.53 ppm for N-(2-Chloroallyl)-1-(R)-aminoindan (Chloro impurity) with a correlation coefficient 0.9973. Limit of detection and limit of quantitation was found to be 0.08 ppm and 0.23 ppm respectively. Recovery for this impurity was found between 92.75% and 102.49%. Method was found to be specific, selective, precise, and robust. The developed method can successfully be applied for the determination of Chloro impurity in Rasagiline Mesylate upto very low trace level concnetration.
New stability indicating reverse phase high performance liquid chromatography (HPLC) method is de... more New stability indicating reverse phase high performance liquid chromatography (HPLC) method is developed for the determination of Imiquimod and its impurities. Separation is achieved on a C18 column (Inertsil-ODS3 4.6 × 250 mm, 5 µm) using gradient elution mode with mobile phase-A having disodium hydrogen phosphate buffer (10 mM) with 0.1% v/v triethyl amine and pH adjusted to 6.0 with ortho-phosphoric acid while mobile phase-B consist of an equal mixture of methanol and acetonitrile. The flow rate was optimized to 1.2 mL/min and column oven temperature 30°C. Detection was carried out at wavelength 226 nm. This developed method is then validated as per International Council for Harmonisation (ICH) guideline and found out to be linear, accurate, specific, selective, precise, and robust. The drug is also subjected to forced degradation using Original Research Article
UPLC is an advance technique of liquid chromatography where it takes advantage of innovation in v... more UPLC is an advance technique of liquid chromatography where it takes advantage of innovation in various technologies such as instrumentation and particle size to achieve dramatic increases in resolution, speed and sensitivity of the liquid chromatography. It operates at higher pressure than that used in HPLC and uses fine particles (less than 2.5µm) & mobile phases at high linear velocities. UPLC Technology is now applied throughout the world produce quality data with reproducible and robust methods as compared to the conventional HPLC. UPLC can be hyphenated with other techniques such as Mass spectrometer (MS), Ion chromatograph (IC), Nuclear magnetic resonance spectrometer (NMR) and Infrared spectrometer (IR) etc. This technique provides unique end-to-end solutions for all industries and has found application in various fields such as pharmaceutical, food, environmental, forensic, toxicology and pesticide.
Nitrosamine impurities are known to be mutagenic and carcinogenic, very small exposure of these i... more Nitrosamine impurities are known to be mutagenic and carcinogenic, very small exposure of these impurities can lead to cancer. These impurities may be formed and get incorporated into drug substance or drug product through reagent, catalyst, solvent or raw materials used in the process of manufacturing. The various regulatory authority has published the press release or notice regarding the control of these impurities with the interim limit. Nitrosamine impurities can be avoided by taking precaution in the manufacturing of drug substance and drug products. Validated analytical methods are to be used to identify and quantify these impurities hence it needs highly sensitive instrument which can detect these impurities to the trace level at given interim limit. Liquid chromatography or Gas chromatography, along with mass detector is majorly used for their determination.
Impurities are unwanted chemical substances present in the Pharmaceutical drug products and drug ... more Impurities are unwanted chemical substances present in the Pharmaceutical drug products and drug substances with no therapeutic benefits or some time potential to harm patient safety if present above a certain limit. The basic need in manufacturing of safe and good quality of drug substances and drug product, control of impurities is very necessary for the pharmaceutical industry. Several regulatory agencies have formulated guidelines for the control of these impurities. The present review article describes the impurities, origin of impurities, classification of impurities, control limit of impurities, guidelines for their control, isolation of impurities and its characterization using various analytical techniques.
Environmental pollution is majorly caused by the chemical and pharmaceutical industries which hav... more Environmental pollution is majorly caused by the chemical and pharmaceutical industries which have increased multifold time in the last several decades. It is the responsibility of science to design the process which will generate the less hazardous chemicals and much environmentally friendly waste. Ionic liquid finds a source of hope in reducing the organic solvent waste in coming years. These Ionic liquids may replace the organic solvents which are hazardous, toxic and non-environmentally friendly used in the synthesis of chemical compounds. This review article describes the Introduction to Ionic liquids, their types and classification, the advantages of their use in replacement of organic solvent in the synthesis of chemicals compounds and drug substances.
A rapid, sensitive and highly selective High performance liquid chromatography (HPLC) method was ... more A rapid, sensitive and highly selective High performance liquid chromatography (HPLC) method was developed and validated for the determination of trace level Genotoxic Melamine impurity, as required by USFDA and that may be present in Allopurinol. HPLC column used was Cosmosil C18 (250 x 4.6 mm, 5µm). The isocratic elution modewas selected where the mobile phaseconsists of 1.25 g/l Sodium dihydrogen phosphate solution. The flow rate was set to1.0 mL/minand run time of 30 minutes. UV detector with wavelength 208 nm was used for theanalysis. The column oven temperature was kept at 25°C. The developed method was validated according to ICH guideline and found to be linear in the range of 5.20 ppm to 52.05 ppm with a correlation coefficient 0.9997. Limit of detection and limit of quantitation was found to be 1.21 ppm and 3.68 ppm respectively. Recovery for this impurity was found between 93.37% and 107.59%.A method was found to be specific, selective, precise, and robust. The developed method can successfully be applied for the determination of Genotoxic Melamine impurity in Allopurinol.
A simple, precise, linear, accurate and robust spectrophotometric method was developed for the es... more A simple, precise, linear, accurate and robust spectrophotometric method was developed for the estimation of palladium content in Rasagiline Mesylate. The proposed method is based on complex formation of palladium with α-nitroso-β-napthol in alkaline medium and extraction with toluene and estimation. The spectrum shows maximum absorption at 425 nm. The method is validated as per on International council for harmonization (ICH) guidelines. The absorbance-concentration plot is linear over the concentration range of 3.08 to15.38 ppm with limit of detection (LOD) of 0.06 ppm and limit of quantification (LOQ) of 0.17 ppm. The recovery of Palladium in Rasagiline Mesylate obtained was between 95 to 105 %. The proposed method can be applied for the determination of palladium content in Rasagiline Mesylate. Original Research Article Hussain et al.; BJPR, 15(4): 1-7, 2017; Article no.BJPR.32254 2
A rapid, sensitive and selective High performance liquid chromatography (HPLC) method was develop... more A rapid, sensitive and selective High performance liquid chromatography (HPLC) method was developed and validated for the trace analysis of N-(2-Chloroallyl)-1-(R)-aminoindan, a potential genotoxic impurity in Rasagiline mesylate drug substances. HPLC column used was Sunfire C18 (250 mm x 4.6 mm, 5 μm). The gradient elution mode was selected where mobile phase-A consist of Buffer (40Mm Ammonium dihydrogen phosphate solution adjusted to pH 7.0 with orthophosphoric acid) and mobile phase-B in 60:40 ratio, whereas mobile phase B consist of solvent Acetonitrile and Methanol in the ratio 70:30. The flow rate was set to 1.5 mL/min and run time of 35 minutes. UV detector with wavelength 210 nm was used for the analysis. Column oven temperature was kept 40°C. The developed method was validated according ICH guideline and found to be linear in the range of 0.51 ppm to 1.53 ppm for N-(2-Chloroallyl)-1-(R)-aminoindan (Chloro impurity) with a correlation coefficient 0.9973. Limit of detection and limit of quantitation was found to be 0.08 ppm and 0.23 ppm respectively. Recovery for this impurity was found between 92.75% and 102.49%. Method was found to be specific, selective, precise, and robust. The developed method can successfully be applied for the determination of Chloro impurity in Rasagiline Mesylate upto very low trace level concnetration.
New stability indicating reverse phase high performance liquid chromatography (HPLC) method is de... more New stability indicating reverse phase high performance liquid chromatography (HPLC) method is developed for the determination of Imiquimod and its impurities. Separation is achieved on a C18 column (Inertsil-ODS3 4.6 × 250 mm, 5 µm) using gradient elution mode with mobile phase-A having disodium hydrogen phosphate buffer (10 mM) with 0.1% v/v triethyl amine and pH adjusted to 6.0 with ortho-phosphoric acid while mobile phase-B consist of an equal mixture of methanol and acetonitrile. The flow rate was optimized to 1.2 mL/min and column oven temperature 30°C. Detection was carried out at wavelength 226 nm. This developed method is then validated as per International Council for Harmonisation (ICH) guideline and found out to be linear, accurate, specific, selective, precise, and robust. The drug is also subjected to forced degradation using Original Research Article
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