邻菲啰啉-Fe(Ⅱ)光度法间接测定药物中乙酰半胱氨酸含量
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摘要
建立了邻菲啰啉-Fe(Ⅱ)光度法间接测定乙酰半胱氨酸含量的新方法。利用乙酰半胱氨酸分子中的巯基(—SH)可将Fe(Ⅲ)还原为Fe(Ⅱ),Fe(Ⅱ)与邻菲啰啉反应生成在510nm处有最大吸收的稳定橙红色络合物,通过测定橙红色络合物的吸光度,可间接测定乙酰半胱氨酸的含量。结果表明,乙酰半胱氨酸质量浓度在0.800 0~5.600μg/mL范围内与吸光度A呈良好的线性关系,线性回归方程为A=-0.066 9+153.17c,线性相关系数r=0.999 7。方法用于实际药品中乙酰半胱氨酸的含量测定,结果与药典法一致。
A novel method for the indirect determination of acetylcysteine by spectrophotometry using phenanthroline-Fe(Ⅱ)was established.Fe(Ш)was reduced to Fe(Ⅱ)by hydrosulfuryl(—SH)in acetylcysteine molecule,and then Fe(Ⅱ)reacted with phenanthroline to form a stable orange red complex with absorption wavelength at 510 nm.The content of acetylcysteine was determinated indirectly through measuring the absorbance of the stable orange red complex.The results showed that a good linear relationship was obtained between the absorbance and the concentration of acetylcysteine in the range of0.800 0~5.600μg/mL.The equation of the linear regression was A=-0.066 9+153.17 c,with a linear correlation coefficient of 0.999 7.This proposed method has been applied to determinate acetylcysteine in real pharmaceuticals,and the results agree well with those from pharmacopoeial method.
A novel method for the indirect determination of acetylcysteine by spectrophotometry using phenanthroline-Fe(Ⅱ)was established.Fe(Ш)was reduced to Fe(Ⅱ)by hydrosulfuryl(—SH)in acetylcysteine molecule,and then Fe(Ⅱ)reacted with phenanthroline to form a stable orange red complex with absorption wavelength at 510 nm.The content of acetylcysteine was determinated indirectly through measuring the absorbance of the stable orange red complex.The results showed that a good linear relationship was obtained between the absorbance and the concentration of acetylcysteine in the range of0.800 0~5.600μg/mL.The equation of the linear regression was A=-0.066 9+153.17 c,with a linear correlation coefficient of 0.999 7.This proposed method has been applied to determinate acetylcysteine in real pharmaceuticals,and the results agree well with those from pharmacopoeial method.
引文
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[9]SHAIDAROVA L G,GEDMINA A V,ZHALDAKE R,et al.Voltammetric Determination of Acetylcysteine in Drugs Using an Electrode Modified by an Osmium Hexacyanocobaltate Film[J].Pharm Chem J,2014,47(12):670-674.
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[11]WU X M,JI Y.Determination of Acetylcysteine and Acetyltyrosine in Compound Amino Acid Injection by RP-HPLC[J].Chin J Biochem Pharm,2003,24(4):194-195(in Chinese).(吴小曼,纪宇.反相高效液相色谱法测定复方氨基酸注射液中的乙酰半胱氨酸和乙酰酪氨酸[J].中国生化药物杂志,2003,24(4):194-195.)
[12]XI J J,WANG F G,ZHUANG R X,et al.Determination of Acetylcysteine in Rabbit Plasma by RP-HPLC[J].China Pharm,2012,21(5):13-14(in Chinese).(席建军,王福根,庄让笑,等.反相高效液相色谱法测定家兔体内乙酰半胱氨酸血药浓度[J].中国药业,2012,21(5):13-14.)
[2]Chinese Pharmacopoeia Commission.Pharmacopoeia of People’s Republic of China(2010edition,two)[M].Beijing:China Medical Science Press,2010:5(in Chinese).(国家药典委员会.中华人民共和国药典(2010年版,二部)[M].北京:中国医药科技出版社,2010:5.)
[3]MAHER A E.Spectrophotometric Determination of Cysteine and N-acetylcysteine in Pharmaceutical Preparations[J].Microchim Acta,1998,129(1-2):91-95.
[4]SUAREZ W T,MADI A A,VICENTINI F C,et al.Flow-Injection Spectrophotometric Determination of N-acetylcysteine in Pharmaceutical Formulations with On-Line Solid-Phase Reactor Containing Zn(Ⅱ)Phosphate Immobilized in a Polyester Resin[J].Anal Lett,2007,40(18):3 417-3 429.
[5]ZHANG S H.Flowinjection Analysis for Determination of N-acetylcysteine in Injection of 17Amino Acid[J].Chin Pharm J,1994,29(4):219-221(in Chinese).(张少辉.流动注射分析测定十七合氨基酸输液中乙酞半眯氨酸含量[J].中国药学杂志,1994,29(4):219-221.)
[6]LI H,YANG Y M.Determination of Acetylcysteine in Luminol-Cu(Ⅱ)System by Flow Injection Chemiluminescence[J].Chin J Spectrosc Lab,2010,27(5):1 968-1 970(in Chinese).(李红,杨育民.Luminol-Cu(Ⅱ)体系流动注射化学发光法测定乙酰半胱氨酸[J].光谱实验室,2010,27(5):1 968-1 970.)
[7]PATSOUKIS N,GEORGIOU C D.Fluorometric Determination of Thiol Redox State[J].Anal Bioanal Chem,2005,383(6):923-929.
[8]YANG X H,JING B B,ZHANG S H,et al.Fluorimetric Determination of Acetylcysteine Bace on Calcein-Copper(Ⅱ)System[J].Prog Mod Biomed,2011,11(7):1 355-1 358(in Chinese).(杨晓红景蓓蓓张胜海,等.基于钙黄绿素-铜(Ⅱ)荧光体系测定乙酰半胱氨酸[J].现代生物医学进展,2011,11(7):1 355-1 358.)
[9]SHAIDAROVA L G,GEDMINA A V,ZHALDAKE R,et al.Voltammetric Determination of Acetylcysteine in Drugs Using an Electrode Modified by an Osmium Hexacyanocobaltate Film[J].Pharm Chem J,2014,47(12):670-674.
[10]RAOOF J B,OJANI R,AMIRI A M,et al.Catechol as an Electrochemical Indicator for Voltammetric Determination of N-acetyl-l-cysteine in Aqueous Media at the Surface of Carbon Paste Electrode[J].JAppl Electrochem,2010,40(7):1 357-1 363.
[11]WU X M,JI Y.Determination of Acetylcysteine and Acetyltyrosine in Compound Amino Acid Injection by RP-HPLC[J].Chin J Biochem Pharm,2003,24(4):194-195(in Chinese).(吴小曼,纪宇.反相高效液相色谱法测定复方氨基酸注射液中的乙酰半胱氨酸和乙酰酪氨酸[J].中国生化药物杂志,2003,24(4):194-195.)
[12]XI J J,WANG F G,ZHUANG R X,et al.Determination of Acetylcysteine in Rabbit Plasma by RP-HPLC[J].China Pharm,2012,21(5):13-14(in Chinese).(席建军,王福根,庄让笑,等.反相高效液相色谱法测定家兔体内乙酰半胱氨酸血药浓度[J].中国药业,2012,21(5):13-14.)