Based on the absorption property of a diazine that can be formed by reaction of glyoxal and 3-methyl-2-benzothiazolinone hydrazone(MBTH)in the Ultravioletvisible(UV-vis)spectral region,a HPLC method was developed for ...Based on the absorption property of a diazine that can be formed by reaction of glyoxal and 3-methyl-2-benzothiazolinone hydrazone(MBTH)in the Ultravioletvisible(UV-vis)spectral region,a HPLC method was developed for the determination of glyoxal in acetaldehyde solution.Glyoxal was derivatised from MBTH and the derivatives(diazine)were analyzed by HPLC for identification and quantification.The determination was performed on a ZORBAX Eclipse XDB-C18 column(4.6250 mm,5 mm)at 35℃ with an injection volume of 10 mL,using a mixture of acetonitrile-water solvent(99∶5,v∶v)as a mobile phase with a flow rate of 0.8 mL·min^(–1).The proper derivative reaction conditions were the temperature of 70℃,MBTH to carbonyl molar ratio of 12,and reaction time of 110 min.The glyoxal diazine was a yellow dye with a maximum molar absorptivity at 401 nm and its retention time was 5.2 min under optimal HPLC conditions.The standard curve for glyoxal had a strong linear relationship with a regression coefficient(R2=0.999)in the range of 0.002–0.020 g·L^(–1).The analysis of glyoxal in an oxidising solution gave accurate results with a relative standard deviation(RSD)value of 0.55%.The average relative recovery was 102%.This efficient HPLC technique is also proposed for detecting other dicarbonyl compounds besides glyoxal.展开更多
Two simple, rapid, sensitive, accurate, precise and economical Visible Spectrophotometric methods have been developed for the determination of Etravirine in pure and pharmaceutical formulations. These methods (A and B...Two simple, rapid, sensitive, accurate, precise and economical Visible Spectrophotometric methods have been developed for the determination of Etravirine in pure and pharmaceutical formulations. These methods (A and B) were based on nucleophilic substitution and oxidative coupling reactions of Etravirine by 1,2-naphtha quinone-4-sulphonate (NQS) in alkaline medium and 3-methyl-2-benzothiazolinone hydrazone (MBTH) in acidic medium with the maximum absorbance at 414 nm and 635 nm respectively. Linearity was obtained in the concentration range of 5 -30 μg/ml and 2 -10 μg/ml which was corroborated by the correlation coefficient (r) values of 0.9995 and 0.9996 respectively. The methods developed were validated with respect to linearity, accuracy (recovery), precision, Sandell’s sensitivity, molar extinction coefficient and specificity. The proposed methods are successfully applied for the determination of Etravirine in bulk and pharmaceutical formulations and results were validated statistically by recovery studies.展开更多
基金Financial support by the China Petroleum and Chemical Corporation is gratefully acknowledged.
文摘Based on the absorption property of a diazine that can be formed by reaction of glyoxal and 3-methyl-2-benzothiazolinone hydrazone(MBTH)in the Ultravioletvisible(UV-vis)spectral region,a HPLC method was developed for the determination of glyoxal in acetaldehyde solution.Glyoxal was derivatised from MBTH and the derivatives(diazine)were analyzed by HPLC for identification and quantification.The determination was performed on a ZORBAX Eclipse XDB-C18 column(4.6250 mm,5 mm)at 35℃ with an injection volume of 10 mL,using a mixture of acetonitrile-water solvent(99∶5,v∶v)as a mobile phase with a flow rate of 0.8 mL·min^(–1).The proper derivative reaction conditions were the temperature of 70℃,MBTH to carbonyl molar ratio of 12,and reaction time of 110 min.The glyoxal diazine was a yellow dye with a maximum molar absorptivity at 401 nm and its retention time was 5.2 min under optimal HPLC conditions.The standard curve for glyoxal had a strong linear relationship with a regression coefficient(R2=0.999)in the range of 0.002–0.020 g·L^(–1).The analysis of glyoxal in an oxidising solution gave accurate results with a relative standard deviation(RSD)value of 0.55%.The average relative recovery was 102%.This efficient HPLC technique is also proposed for detecting other dicarbonyl compounds besides glyoxal.
文摘Two simple, rapid, sensitive, accurate, precise and economical Visible Spectrophotometric methods have been developed for the determination of Etravirine in pure and pharmaceutical formulations. These methods (A and B) were based on nucleophilic substitution and oxidative coupling reactions of Etravirine by 1,2-naphtha quinone-4-sulphonate (NQS) in alkaline medium and 3-methyl-2-benzothiazolinone hydrazone (MBTH) in acidic medium with the maximum absorbance at 414 nm and 635 nm respectively. Linearity was obtained in the concentration range of 5 -30 μg/ml and 2 -10 μg/ml which was corroborated by the correlation coefficient (r) values of 0.9995 and 0.9996 respectively. The methods developed were validated with respect to linearity, accuracy (recovery), precision, Sandell’s sensitivity, molar extinction coefficient and specificity. The proposed methods are successfully applied for the determination of Etravirine in bulk and pharmaceutical formulations and results were validated statistically by recovery studies.
