MSPE-HPLC测定蒲地蓝口服液中咖啡酸和阿魏酸含量
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摘要
建立一种快速且高效的用于蒲地蓝口服液中的咖啡酸和阿魏酸含量测定磁固相萃取-高效液相色谱(MSPE-HPLC)法。采用磁性Mg-Al层状双金属氢氧化物(Mg-Al LDHs)作为吸附剂,利用磁固相萃取分离富集蒲地口服液中咖啡酸和阿魏酸,并利用高效液相色谱法测定咖啡酸和阿魏酸含量。结果表明咖啡酸的最大富集倍数可达24.9倍,阿魏酸最大富集倍数可达21.9倍。MSPE过程的最佳工艺为:吸附时间6min、萃取温度为35℃、样品溶液pH为7.0,解吸溶液pH为2.0、萃取剂用量为4.0 mg。在最佳室验条件下,样品的回收率分别为咖啡酸97.42%～98.57%,阿魏酸96.32%～97.84%。咖啡酸RSD为1.72%,阿魏酸RSD为2.67%。本文所建立的以磁性双金属氢氧化物为吸附剂的MSPE-HPLC法,前处理快速简便,无需特别装置,试剂用量少,对于环境污染小,可以实现蒲地蓝消炎口服液中咖啡酸和阿魏酸的同时测定。
To establish a rapid and efficient method for the determination of caffeic acid and ferulic acid in Pu Dilan oral liquid by MSPE-HPLC.The response surface method was used to determine the best MSPE.The magnetic Mg-Al LDHs was used as adsorbent to separate and enrich caffeic acid and ferulic acid in pudilan oral liquid by magnetic solid phase extraction.The results showed that the maximum enrichment ratio of caffeic acid was 24.9 times and that of ferulic acid was 21.9 times.The optimal process for the MSPE process was as follows:adsorption time was 6 min,extraction temperature was 35 ℃,pH of sample solution was 7.0,pH of desorption solution was 2.0,and extraction agent dosage was 4.0 mg.The recovery rates of the samples were 97.42%～98.57% and 96.32%～97.84%.respectively.At the same time,the samples of different pu dilan oral liquid were measured,and the calculated RSD of caffeic acid was 1.72%,and that of ferulic acid was 2.67%.The MSPE-HPLC method based on magnetic bimetal hydride as adsorbent is rapid and simple in pretreatment,without special device,with low reagent dosage and little environmental pollution.
To establish a rapid and efficient method for the determination of caffeic acid and ferulic acid in Pu Dilan oral liquid by MSPE-HPLC.The response surface method was used to determine the best MSPE.The magnetic Mg-Al LDHs was used as adsorbent to separate and enrich caffeic acid and ferulic acid in pudilan oral liquid by magnetic solid phase extraction.The results showed that the maximum enrichment ratio of caffeic acid was 24.9 times and that of ferulic acid was 21.9 times.The optimal process for the MSPE process was as follows:adsorption time was 6 min,extraction temperature was 35 ℃,pH of sample solution was 7.0,pH of desorption solution was 2.0,and extraction agent dosage was 4.0 mg.The recovery rates of the samples were 97.42%～98.57% and 96.32%～97.84%.respectively.At the same time,the samples of different pu dilan oral liquid were measured,and the calculated RSD of caffeic acid was 1.72%,and that of ferulic acid was 2.67%.The MSPE-HPLC method based on magnetic bimetal hydride as adsorbent is rapid and simple in pretreatment,without special device,with low reagent dosage and little environmental pollution.
引文
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[7]Lin Hao,Xing-Li Liu,Jun-Tao Wang,et al.Metal-organic framework derived magnetic nanoporous carbon as an adsorbent for the magnetic solid-phase extraction of chlorophenols from mushroom sample[J].Chinese Chemical Letters,2016,27(5):783-788.
[8]Mohammad Saraji,Milad Ghani.Dissolvable layered double hydroxide coated magnetic nanoparticlesfor extraction followed by high performance liquid chromatographyfor the determination of phenolic acids in fruit juices[J].J Chromatography A,2014,1366:24-30.
[9]Hossein Abdolmohammad-Zadeh,ZeynabTalleb.Speciation of As(III)/As(V)in water samples by a magnetic solid phase extraction based on Fe3O4/Mg–Al layered double hydroxide nano-hybrid followed by chemiluminescence detection[J].Talanta,2014,128:147-155.
[10]董自波,李超,邵建国.HPLC同时测定蒲地蓝消炎口服液中7个成分的含量[J].中国中药杂志,2015,40(9):1747-1750.
[2]Li Y L,Yan Y,Tan Y F,et al.Qualitative fingerprint and quantitative determination of caffeic acid in compound dandelion enema[J].Nan Fang Yi Ke Da Xue Xue Bao,2006,26(10):1503-1505.
[3]Alinezhad H,Amiri A,Tarahomi M,et al.Magnetic solid-phase extraction of non-steroidal anti-inflammatory drugs from environmental water samples using polyamidoamine dendrimer functionalized with magnetite nanoparticles as a sorbent.[J].Talanta,2018,183:149-157.
[4]Ren K,Zhang W,Cao S,et al.Carbon-based Fe3O4 nanocomposites derived from waste pomelo peels for magnetic solid-phase extraction of 11 triazole fungicides in fruit samples[J].Nanomaterials(Basel),2018;8(5),302-305.
[5]Lin Hao,Xing-Li Liu,Jun-Tao Wang,et al.Metal-organic framework derived magnetic nanoporous carbon as an adsorbent for the magnetic solid-phase extraction of chlorophenols from mushroom sample[J].Chinese Chemical Letters,2016,27(5):783-788.
[6]Tang S,Chia GH,Chang Y,et al.Automated dispersive solid-phase extraction using dissolvable Fe3O4-layered double hydroxide core-shell microspheres as sorbent[J].Anal Chem,2014,86(22):11070-11076.
[7]Lin Hao,Xing-Li Liu,Jun-Tao Wang,et al.Metal-organic framework derived magnetic nanoporous carbon as an adsorbent for the magnetic solid-phase extraction of chlorophenols from mushroom sample[J].Chinese Chemical Letters,2016,27(5):783-788.
[8]Mohammad Saraji,Milad Ghani.Dissolvable layered double hydroxide coated magnetic nanoparticlesfor extraction followed by high performance liquid chromatographyfor the determination of phenolic acids in fruit juices[J].J Chromatography A,2014,1366:24-30.
[9]Hossein Abdolmohammad-Zadeh,ZeynabTalleb.Speciation of As(III)/As(V)in water samples by a magnetic solid phase extraction based on Fe3O4/Mg–Al layered double hydroxide nano-hybrid followed by chemiluminescence detection[J].Talanta,2014,128:147-155.
[10]董自波,李超,邵建国.HPLC同时测定蒲地蓝消炎口服液中7个成分的含量[J].中国中药杂志,2015,40(9):1747-1750.
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