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DOI: 10.6084/m9.figshare.3381337
title: Method development and photolytic degradation study of doxofylline by rp-hplc and lc-msms.

description: A simple, rapid and accurate RP-HPLC method was developed for the determination of doxofylline and photolytic degradation product. The method showed a linearresponse for concentrations in the range of 1-200 ìg/ml using acetonitrile: formic acid (90: 10); pH-3.0 as the mobile phase with detection at 274 nm and a flow rateof 1 ml/min and retention time 2.9 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solutionstability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be lessthan 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis. The photolytic degradation product as well as pathway was characterized by LC-MS/MS.RESULT AND DISCUSSIONA sensitive, selective, precise and accurate highperformance liquid chromatographic method ofanalysis of doxofylline in both as bulk drug and in formulation was developed and validated. The mobile phase consisted of acetonitril:0.05M formic Acid (90: 10v/v); pH-3.0. The detection wavelength was 274nm. Thissystem was found to give the sharp peak for doxofylline (RT-2.9). The method was validated as per ICH guideline. Stability indicating assay method in which photolyticstress condition was used for quantitative estimation of doxofylline in tablet formulation and identification of photolytic degradation product The separation of drug from its degradation product were optimized by varying the ratio &/or nature of organic modifier. Finally method was developed using same mobile phase composed of acetonitrile: formic acid (90: 10); pH-3.0, in that both drug and degradation product showing good elutionRT-2.9 (Doxofylline) and RT-4.7 (Photolytic degradation product) and m/e-413 (Dimer).The photolytic degradation product and pure drug were identified by LC-MS/MS in order to establish photolytic degradation pathway.<br>
DOI: 10.6084/m9.figshare.3381337.v1
title: Method development and photolytic degradation study of doxofylline by rp-hplc and lc-msms.

description: A simple, rapid and accurate RP-HPLC method was developed for the determination of doxofylline and photolytic degradation product. The method showed a linearresponse for concentrations in the range of 1-200 ìg/ml using acetonitrile: formic acid (90: 10); pH-3.0 as the mobile phase with detection at 274 nm and a flow rateof 1 ml/min and retention time 2.9 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solutionstability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be lessthan 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis. The photolytic degradation product as well as pathway was characterized by LC-MS/MS.RESULT AND DISCUSSIONA sensitive, selective, precise and accurate highperformance liquid chromatographic method ofanalysis of doxofylline in both as bulk drug and in formulation was developed and validated. The mobile phase consisted of acetonitril:0.05M formic Acid (90: 10v/v); pH-3.0. The detection wavelength was 274nm. Thissystem was found to give the sharp peak for doxofylline (RT-2.9). The method was validated as per ICH guideline. Stability indicating assay method in which photolyticstress condition was used for quantitative estimation of doxofylline in tablet formulation and identification of photolytic degradation product The separation of drug from its degradation product were optimized by varying the ratio &/or nature of organic modifier. Finally method was developed using same mobile phase composed of acetonitrile: formic acid (90: 10); pH-3.0, in that both drug and degradation product showing good elutionRT-2.9 (Doxofylline) and RT-4.7 (Photolytic degradation product) and m/e-413 (Dimer).The photolytic degradation product and pure drug were identified by LC-MS/MS in order to establish photolytic degradation pathway.<br>
DOI: 10.6084/m9.figshare.3381331
title: Synthesis and anti-inflammatory study of novel fluoro-benzothiazole derivatives

description: N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-2-nitrobenzamides; N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-3-nitrobenzamides and N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-4-nitrobenzamides derivatives were synthesized. Sythesised compounds were tested for anti-inflammatory activity bycarrageenin induced rat hind paw edema method compared to standard Diclofenac.Cyclisation Mechanismof BenzothiazoleSince, in 3-chloro -4fluoro aniline, the 2nd and 6th position is the most positive center but 2nd position behave as a more electrophilic centre. As the attack however was on the 2nd position, which is the electrophilic center and it is probable that bromine being as pseudohalogen, behaves as an electrophile by attacking this electrophilic center followed by replacement of hydrogen of 2nd position as one hydrogen bromide while one bromine atom remain attached. Replacement of bromine takes place by attack of thiocyanogen,behaves as a pseudo halogen (electrophile) followed by elimination of potassium bromide. Finally ring closure occur when pH adjusted at pH6 with ammonia and further rearrangement produce 2-amino-6-fluoro-7-chloro-(1, 3)-benzothiazole. Thus the reaction sequence can be as follows.RESULTS AND DISCUSSIONIn the present work, fluorochloroaniline was treated with KSCN in presence of bromine in glacial acetic acid and ammonia to get 2-amino-6-fluro-7-chloro (1, 3)-benzothiazolewith yield around 51%, which was condensed with 2 (3 or 4)- nitrobenzoyl chloride in presence of dry pyridine and acetone to get N-(7-chloro-6-fluoro-1, 3-benzothiazole-2-yl)-2 (3 or 4)-nitrobenzamides with yield around 45-55% . To the above product 2-chloroaniline, 3-chloroaniline, 4-chloroaniline, o-toludine, m-toludine, p-toludine, 2-nitroaniline, 3-nitroaniline, 4-nitroaniline, 2-aminophenol, 3-aminophenol, 4-aminophenol, 2-anisidine, 3-anisidine and 4-anisidine in presence of DMF were treated toget newly synthesized N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-4-nitrobenzamides derivatives through replacing at 7th position chlorine with yield around58-78%. Reaction progress was monitored by thin layer chromatography. All the synthesized compounds of were characterized by melting point, solubility, TLC, IR,1HNMR spectra studies.All the newly synthesized compounds were evaluated for anti-inflammatory activity. Anti-inflammatory activity of synthesized compounds were perform by carrageenininduced rat hind paw edema method on healthy wistar albino rats of either sex weighing between 100-200gm using dose 20 mg/kg body weight (b.w.) for all the synthesizedcompounds as well as for diclofenac as standard.The response to injected carrageenin provides a convenient experimental model of inflammation which has been widely used for evaluating anti-inflammatory drugs.However, from the obtained results by anti-inflammatory activity it found that compound S-7, S-8, S-9, S-202, S-21, S-22 and S-35 exhibited excellent percentage of inhibition as compared to diclofenac.<br>
DOI: 10.6084/m9.figshare.3381331.v1
title: Synthesis and anti-inflammatory study of novel fluoro-benzothiazole derivatives

description: N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-2-nitrobenzamides; N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-3-nitrobenzamides and N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-4-nitrobenzamides derivatives were synthesized. Sythesised compounds were tested for anti-inflammatory activity bycarrageenin induced rat hind paw edema method compared to standard Diclofenac.Cyclisation Mechanismof BenzothiazoleSince, in 3-chloro -4fluoro aniline, the 2nd and 6th position is the most positive center but 2nd position behave as a more electrophilic centre. As the attack however was on the 2nd position, which is the electrophilic center and it is probable that bromine being as pseudohalogen, behaves as an electrophile by attacking this electrophilic center followed by replacement of hydrogen of 2nd position as one hydrogen bromide while one bromine atom remain attached. Replacement of bromine takes place by attack of thiocyanogen,behaves as a pseudo halogen (electrophile) followed by elimination of potassium bromide. Finally ring closure occur when pH adjusted at pH6 with ammonia and further rearrangement produce 2-amino-6-fluoro-7-chloro-(1, 3)-benzothiazole. Thus the reaction sequence can be as follows.RESULTS AND DISCUSSIONIn the present work, fluorochloroaniline was treated with KSCN in presence of bromine in glacial acetic acid and ammonia to get 2-amino-6-fluro-7-chloro (1, 3)-benzothiazolewith yield around 51%, which was condensed with 2 (3 or 4)- nitrobenzoyl chloride in presence of dry pyridine and acetone to get N-(7-chloro-6-fluoro-1, 3-benzothiazole-2-yl)-2 (3 or 4)-nitrobenzamides with yield around 45-55% . To the above product 2-chloroaniline, 3-chloroaniline, 4-chloroaniline, o-toludine, m-toludine, p-toludine, 2-nitroaniline, 3-nitroaniline, 4-nitroaniline, 2-aminophenol, 3-aminophenol, 4-aminophenol, 2-anisidine, 3-anisidine and 4-anisidine in presence of DMF were treated toget newly synthesized N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-4-nitrobenzamides derivatives through replacing at 7th position chlorine with yield around58-78%. Reaction progress was monitored by thin layer chromatography. All the synthesized compounds of were characterized by melting point, solubility, TLC, IR,1HNMR spectra studies.All the newly synthesized compounds were evaluated for anti-inflammatory activity. Anti-inflammatory activity of synthesized compounds were perform by carrageenininduced rat hind paw edema method on healthy wistar albino rats of either sex weighing between 100-200gm using dose 20 mg/kg body weight (b.w.) for all the synthesizedcompounds as well as for diclofenac as standard.The response to injected carrageenin provides a convenient experimental model of inflammation which has been widely used for evaluating anti-inflammatory drugs.However, from the obtained results by anti-inflammatory activity it found that compound S-7, S-8, S-9, S-202, S-21, S-22 and S-35 exhibited excellent percentage of inhibition as compared to diclofenac.<br>
DOI: 10.6084/m9.figshare.3381328
title: Eye Tracking Pilot Accuracy and Precision Data

description: This file contains accuracy and precision measurements and raw gaze samples taken from 12 participants in a real-world laboratory setting using Tobii X60, 60Hz Remote Eye Tracker using manufacturer's I-VT filter settings. Stimulus was displayed on a Dell 2209WA flatpanel display monitor at approximately 70cm viewing distance at a resolution of 1680x1050. <br><br> Accuracy data was calculated against fixations on 9 points distributed across upper, middle, lower, left, center, and right thirds of the display. Precision data was calculated against a single fixation for each participant on a non-moving object of focus centered in the display for three seconds' duration, resulting in 80-150 raw gaze samples per participant, dependant on the speed with which the participant was able to focus and fixate on the object.
DOI: 10.6084/m9.figshare.3381322
title: Synthesis and antifungal study of novel fluoro-benzothiazole derivatives

description: N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-2-nitrobenzamides; N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-3-nitrobenzamides and N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-4-nitrobenzamides derivatives were synthesized. The synthesized compounds were screened for antifungal activity at two different concentrations (50μg/ml, 100μg/ml) against Candida albicans and Aspergillus niger by cup plate method (diffusion technique) using Griseoflavin as standard.RESULTAND DISCUSSTIONIn present work, fluorochloro aniline was treated with potassium thiocynate in presence of bromine in glacial acetic acid and ammonia to get 2-amino-6-fluro-7-chloro (1, 3)-benzothiazole which was condensed with 2 (3 or 4)-nitrobenzoylchloride acid in presence of dry pyridine and acetone to get N-(7-chloro-6-fluoro-1, 3-benzothiazole-2-yl)-2 (3 or 4)-nitrobenzamides. To the above product 2-chloroaniline, 3-chloroaniline, 4-chloroaniline, o-toludine,m-toludine, p-toludine, 2-nitroaniline, 3-nitroaniline, 4-nitroaniline, 2- aminophenol, 3-aminophenol, 4-aminophenol, 2-anisidine, 3-anisidine and 4-anisidine in presence of DMF were treated to get newly synthesized N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-4-nitrobenzamides derivatives through replacing at 7th position chlorine. Reaction progress was monitored by thin layer chromatography.Melting points of the synthesized compounds were determined in open capillaries and showed a minute change after recrystallisation. IR spectra (KBr pellet technique) were recorded using a SHIMADZU (8400S), spectrophotometer.
DOI: 10.6084/m9.figshare.3381322.v1
title: Synthesis and antifungal study of novel fluoro-benzothiazole derivatives

description: N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-2-nitrobenzamides; N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-3-nitrobenzamides and N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-4-nitrobenzamides derivatives were synthesized. The synthesized compounds were screened for antifungal activity at two different concentrations (50μg/ml, 100μg/ml) against Candida albicans and Aspergillus niger by cup plate method (diffusion technique) using Griseoflavin as standard.RESULTAND DISCUSSTIONIn present work, fluorochloro aniline was treated with potassium thiocynate in presence of bromine in glacial acetic acid and ammonia to get 2-amino-6-fluro-7-chloro (1, 3)-benzothiazole which was condensed with 2 (3 or 4)-nitrobenzoylchloride acid in presence of dry pyridine and acetone to get N-(7-chloro-6-fluoro-1, 3-benzothiazole-2-yl)-2 (3 or 4)-nitrobenzamides. To the above product 2-chloroaniline, 3-chloroaniline, 4-chloroaniline, o-toludine,m-toludine, p-toludine, 2-nitroaniline, 3-nitroaniline, 4-nitroaniline, 2- aminophenol, 3-aminophenol, 4-aminophenol, 2-anisidine, 3-anisidine and 4-anisidine in presence of DMF were treated to get newly synthesized N-{6-fluoro-7-[(substituted)-amino] 1, 3-benzothiazole-2-yl}-4-nitrobenzamides derivatives through replacing at 7th position chlorine. Reaction progress was monitored by thin layer chromatography.Melting points of the synthesized compounds were determined in open capillaries and showed a minute change after recrystallisation. IR spectra (KBr pellet technique) were recorded using a SHIMADZU (8400S), spectrophotometer.
DOI: 10.6084/m9.figshare.3381316
title: Simultaneous estimation of amoxicillin and potassium clavulanate in injection formulation by dual wavelength spectroscopy

description: A simple, fast and precise dual wavelength method has been developed for simultaneous determination of Amoxycillin (AMX) and Potassium clavulanate (PTC)for injection formulation. The absorption maxima were found 246.6 nm for AMX and 257.6 nm for PTC in 0.5M NaOH used as the solvent. It was found that the absorption maxima of these two drugs were quite close to each other; hence dual wavelength method was selected for their simultaneous estimation. For dual wavelength method two wavelengths selected were 261nm, 226nm and 279nm, 225 nm for AMX and PTC respectively because at these wavelengths drug shows similar absorbance. The developed method was then validated as per ICH guideline.RESULTS AND DISCUSSIONThe UV spectra of AMX and PTC, obtained from different solvent (methanol, water, 0.1mHCl and 0.1M NaOH ) were studied. The wavelength maximum of the main band was found to be dependent of solvent effects. In water ?max found to be 228nm AMX and 222nm for PTC, but theinjection powder was turbid and non filterable. Also the ?max of both drugs found to be very close. In 0.1M HCl drug is freely soluble and ?max found to be 229nm AMX and 224.2nm for PTC but the drug stock solution were dark and yellowish in cololur. In methanol drug is slightly soluble and ?max found to be 232nm AMX and 220.8nm for PTC, but as per solvent effect (Bathochromic shoft ) the ?max of PTC could not be considerable. In case of 0.1M NaOHthe drug is freely soluble and ?max found to be 246.8nm AMX and 257.6nm for PTC. Thus at the end of these studies 0.1M NaOH was selected as best solvent because it fulfill all the parameters required for simultaneous estimation and also to avoid the time gain while preparing solution and cost saving by eliminating the purchase and disposal of organic solvent. After considering the solubility, stability and economic feature for both the drugs, 0.1M NaOH was selected as<br>
DOI: 10.6084/m9.figshare.3381316.v1
title: Simultaneous estimation of amoxicillin and potassium clavulanate in injection formulation by dual wavelength spectroscopy

description: A simple, fast and precise dual wavelength method has been developed for simultaneous determination of Amoxycillin (AMX) and Potassium clavulanate (PTC)for injection formulation. The absorption maxima were found 246.6 nm for AMX and 257.6 nm for PTC in 0.5M NaOH used as the solvent. It was found that the absorption maxima of these two drugs were quite close to each other; hence dual wavelength method was selected for their simultaneous estimation. For dual wavelength method two wavelengths selected were 261nm, 226nm and 279nm, 225 nm for AMX and PTC respectively because at these wavelengths drug shows similar absorbance. The developed method was then validated as per ICH guideline.RESULTS AND DISCUSSIONThe UV spectra of AMX and PTC, obtained from different solvent (methanol, water, 0.1mHCl and 0.1M NaOH ) were studied. The wavelength maximum of the main band was found to be dependent of solvent effects. In water ?max found to be 228nm AMX and 222nm for PTC, but theinjection powder was turbid and non filterable. Also the ?max of both drugs found to be very close. In 0.1M HCl drug is freely soluble and ?max found to be 229nm AMX and 224.2nm for PTC but the drug stock solution were dark and yellowish in cololur. In methanol drug is slightly soluble and ?max found to be 232nm AMX and 220.8nm for PTC, but as per solvent effect (Bathochromic shoft ) the ?max of PTC could not be considerable. In case of 0.1M NaOHthe drug is freely soluble and ?max found to be 246.8nm AMX and 257.6nm for PTC. Thus at the end of these studies 0.1M NaOH was selected as best solvent because it fulfill all the parameters required for simultaneous estimation and also to avoid the time gain while preparing solution and cost saving by eliminating the purchase and disposal of organic solvent. After considering the solubility, stability and economic feature for both the drugs, 0.1M NaOH was selected as<br>
DOI: 10.6084/m9.figshare.3381313
title: Method development and alkali degradation study of doxofylline by rp-hplc and lc-ms/ms

description: response for concentrations in the range of 1-200 ìg/mL using acetonitrile: formic Acid (90: 10); pH-3.0 as the mobile phase with detection at 274 nm and a flow rate of 1 ml/min and retention time 2.9 min. The method was statistically validated for accuracy, precision, linearity, rugge dness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD fromrecovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine qualitycontrol analysis. The acid degradation product as well as pathway was characterized by LC-MS/MS.RESULT AND DISCUSSIONA sensitive, selective, precise and accurate high performance liquid chromatographicmethod of analysis of doxofylline in both as bulk drug and in formulation was developed and validated. The mobile phase consisted of acetonitril: 0.05M formic Acid (90: 10v/v); pH-3.0. The detection wavelength was 274nm. This system was found to give the sharp peak for Doxofylline (RT-2.9). The method was validated as per ICH guideline. Stability indicating assay method in which alkali stress condition was used for quantitative estimation of doxofylline in tablet formulation and identification of alkali degradation product The separation of drug from its degradation product were optimized by varying the ratio &/or nature of organic modifier. Finally method was developed using samemobile phase composed of acetonitrile: formic Acid (90: 10); pH-3.0, in that both drug and degradation product showing good elution RT-2.9 (Doxofylline) and RT-5.1 (Alkalidegradation product) and m/e-262. The acid degradation product and pure drug were identified by LC-MS/MS in order to establish acid degradation pathway(fig.-04, 05and06).
DOI: 10.6084/m9.figshare.3381313.v1
title: Method development and alkali degradation study of doxofylline by rp-hplc and lc-ms/ms

description: response for concentrations in the range of 1-200 ìg/mL using acetonitrile: formic Acid (90: 10); pH-3.0 as the mobile phase with detection at 274 nm and a flow rate of 1 ml/min and retention time 2.9 min. The method was statistically validated for accuracy, precision, linearity, rugge dness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD fromrecovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine qualitycontrol analysis. The acid degradation product as well as pathway was characterized by LC-MS/MS.RESULT AND DISCUSSIONA sensitive, selective, precise and accurate high performance liquid chromatographicmethod of analysis of doxofylline in both as bulk drug and in formulation was developed and validated. The mobile phase consisted of acetonitril: 0.05M formic Acid (90: 10v/v); pH-3.0. The detection wavelength was 274nm. This system was found to give the sharp peak for Doxofylline (RT-2.9). The method was validated as per ICH guideline. Stability indicating assay method in which alkali stress condition was used for quantitative estimation of doxofylline in tablet formulation and identification of alkali degradation product The separation of drug from its degradation product were optimized by varying the ratio &/or nature of organic modifier. Finally method was developed using samemobile phase composed of acetonitrile: formic Acid (90: 10); pH-3.0, in that both drug and degradation product showing good elution RT-2.9 (Doxofylline) and RT-5.1 (Alkalidegradation product) and m/e-262. The acid degradation product and pure drug were identified by LC-MS/MS in order to establish acid degradation pathway(fig.-04, 05and06).
DOI: 10.6084/m9.figshare.3381301
title: Synthesis and cyclization of benzothiazole: review

description: Benzoheterocycles such as benzothiazoles, benzimid azoles and benzoxazoles can serve as unique and versatile scaffolds for experimental drug design. Among the all benzohaterocycles, benzothiazole has considerable place in research area especially in synthetic as well as inpharmaceutical chemistry because of its potent and significant pharmacological activities. Since, awide range of methods are available for synthesizing benzothiazole nucleus and its derivatives but areal need exists for new procedures that support many kinds of structural diversity and varioussubstitution. The present review deals with the common methods adopted and reported to focus thesynthesis as well as cyclisation of benzothiazole nucleus.<br>