基于复红作探针的双波长共振瑞利散射法测定药物中的盐酸米多君
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摘要
以复红为探针建立了快速测定药物中盐酸米多君的高灵敏双波长共振瑞利散射(RRS)法。在pH 3. 46的酸性溶液中,复红与十六烷基溴化吡啶鎓及盐酸米多君作用生成三元离子缔合物,使RRS信号显著增强并产生具有双峰的新的RRS光谱。最大RRS峰位于620 nm,次大RRS峰位于370 nm,在此二波长处的RRS增强强度与0. 009～0. 35 mg/L盐酸米多君的质量浓度呈线性关系,检出限分别为0. 006 2 mg/L(370 nm)和0. 005 8 mg/L(620 nm),当用双波长叠加RRS法测定时,检出限为0. 003 0 mg/L。还研究了三元缔合反应的适宜条件、共存物质的影响及双波长RRS法的光谱特征。该方法可用于市售盐酸米多君药片中盐酸米多君含量的测定,回收率和相对标准偏差RSD%(n=5)分别为98. 3%～102%和1. 2%～1. 8%。
A new highly sensitive dual-wavelength resonance Rayleigh scattering( RRS) method for rapid determination of midodrine hydrochloride in drugs is established with fuchsin as probe.In an acidic solution of pH 3. 46,fuchsin reacts with 1-hexadecylpyridinium bromide and midodrine hydrochloride to form a ternary ion association complex,which leads to a greatly enhanced resonance Rayleigh scattering( RRS) signal of system and produces a new RRS spectrum with double peaks.The largest RRS peak locates at 620 nm and the second largest RRS peak locates at 370 nm.At these two wavelengths,RRS enhanced intensity( ΔIRRS) is directly proportional to the mass concentration of midodrine hydrochloride in the range of 0. 009 to 0. 35 mg·L~(-1). The detection limits are 0. 006 2 mg·L~(-1)( for 370 nm peak) and 0. 005 8 mg·L~(-1)( for 620 nm peak),respectively.When dual-wavelength superposition RRS method is used to determine the concentrations of midodrine hydrochloride,the detection limit is 0. 003 0 mg·L~(-1). The suitable conditions for the ternary association reaction,the influence of coexisting substances and the spectral characteristics of dualwavelength RRS method are also studied. This method can be applied to the determination content of midodrine hydrochloride in commercially available midodrine hydrochloride tablets with the recoveries in the range of 98. 3% to102% and RSD%( n = 5) between 1. 2% and 1. 8%.
A new highly sensitive dual-wavelength resonance Rayleigh scattering( RRS) method for rapid determination of midodrine hydrochloride in drugs is established with fuchsin as probe.In an acidic solution of pH 3. 46,fuchsin reacts with 1-hexadecylpyridinium bromide and midodrine hydrochloride to form a ternary ion association complex,which leads to a greatly enhanced resonance Rayleigh scattering( RRS) signal of system and produces a new RRS spectrum with double peaks.The largest RRS peak locates at 620 nm and the second largest RRS peak locates at 370 nm.At these two wavelengths,RRS enhanced intensity( ΔIRRS) is directly proportional to the mass concentration of midodrine hydrochloride in the range of 0. 009 to 0. 35 mg·L~(-1). The detection limits are 0. 006 2 mg·L~(-1)( for 370 nm peak) and 0. 005 8 mg·L~(-1)( for 620 nm peak),respectively.When dual-wavelength superposition RRS method is used to determine the concentrations of midodrine hydrochloride,the detection limit is 0. 003 0 mg·L~(-1). The suitable conditions for the ternary association reaction,the influence of coexisting substances and the spectral characteristics of dualwavelength RRS method are also studied. This method can be applied to the determination content of midodrine hydrochloride in commercially available midodrine hydrochloride tablets with the recoveries in the range of 98. 3% to102% and RSD%( n = 5) between 1. 2% and 1. 8%.
引文
[1]安明,赵国君,王国成,等.毛细管色谱法测定盐酸米多君中的有机溶剂残留量[J].沈阳药科大学学报,2012,29(2):136-138.
[2]唐跃林,江舸.盐酸米多君原料药含量测定方法的改进[J].四川生理科学杂志,2016,38(2):59-61.
[3]Sneha G N,Jaivik V S,Priyanka A S,et al.Extractive spectrophotometric determination of five selected drugs by ion-pair complex formation with bromothymol blue in pure form and pharmaceutical preparations[J].Cogent Chemistry,2015,1(1):54-60.
[4]王金山.盐酸米多君片溶出度测定法的研究[J].海峡药学,2009,21(7):94-97.
[5]中华人民共和国药典委员会.中华人民共和国药典(二部)[M].北京:中国医药科技出版社,2015:962.
[6]Barth T,Aleu J,Pupo M T,et al.HPLC analysis of midodrine and desglymidodrine in culture medium:Evaluation of static and shaken conditions on the biotransformation by fungi[J].Journal of Chromatographic Science,2013,51(5):460-466.
[7]Yoshida H,Ohno Y,Yoshikuni K,et al.Determination of midodrine in human plasma by high-performance liquid chromatography with fluorescence detection[J].Analytical Sciences(Print),2003,19(2):317-325.
[8]Daxesh P P,Sneha N,Bhanubhai N S,et al.A novel,sensitive and selective method of UPLC/MS-MS for rapid simultaneous determination of midodrine and its active metabolite desglymidodrine in human plasma:Application to support bioequivalence study in healthy human volunteers[J].Journal of Pharmaceutical and Biomedical A-nalysis,2016,131:355-363.
[9]Ahmed A A,Medhat A A G,Samar F F,et al.Development and validation of LC-MS/MS assay for the determination of the prodrug midodrine and its active metabolite desglymidodrine in plasma of ascitic patients:Application to individualized therapy and comparative pharmacokinetics[J].Journal of Chromatography B,2015,991:34-40.
[2]唐跃林,江舸.盐酸米多君原料药含量测定方法的改进[J].四川生理科学杂志,2016,38(2):59-61.
[3]Sneha G N,Jaivik V S,Priyanka A S,et al.Extractive spectrophotometric determination of five selected drugs by ion-pair complex formation with bromothymol blue in pure form and pharmaceutical preparations[J].Cogent Chemistry,2015,1(1):54-60.
[4]王金山.盐酸米多君片溶出度测定法的研究[J].海峡药学,2009,21(7):94-97.
[5]中华人民共和国药典委员会.中华人民共和国药典(二部)[M].北京:中国医药科技出版社,2015:962.
[6]Barth T,Aleu J,Pupo M T,et al.HPLC analysis of midodrine and desglymidodrine in culture medium:Evaluation of static and shaken conditions on the biotransformation by fungi[J].Journal of Chromatographic Science,2013,51(5):460-466.
[7]Yoshida H,Ohno Y,Yoshikuni K,et al.Determination of midodrine in human plasma by high-performance liquid chromatography with fluorescence detection[J].Analytical Sciences(Print),2003,19(2):317-325.
[8]Daxesh P P,Sneha N,Bhanubhai N S,et al.A novel,sensitive and selective method of UPLC/MS-MS for rapid simultaneous determination of midodrine and its active metabolite desglymidodrine in human plasma:Application to support bioequivalence study in healthy human volunteers[J].Journal of Pharmaceutical and Biomedical A-nalysis,2016,131:355-363.
[9]Ahmed A A,Medhat A A G,Samar F F,et al.Development and validation of LC-MS/MS assay for the determination of the prodrug midodrine and its active metabolite desglymidodrine in plasma of ascitic patients:Application to individualized therapy and comparative pharmacokinetics[J].Journal of Chromatography B,2015,991:34-40.