流动注射化学发光法在抗生素药物分析中的研究与应用
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摘要
化学发光(Chemiluminescence,简称CL)是化学反应中由于化学能的转移,使反应物激发到激发态,激发态物质跃回基态时释放能量产生光辐射的过程。流动注射分析(Flow-injection analysis,简称FIA)是指在具有流速的载流中,试样与试剂反应能高度重现定量分析技术。将化学发光与流动注射相结合,形成的流动注射化学发光分析法具有灵敏度高、线性范围广、分析速度快、仪器简单及易于实现自动化等特点,广泛地应用于生物医药、环境监测、食品卫生和材料分析等领域。本论文基于药物对鲁米诺体系具有增敏或抑制作用,主要进行了以下几个方面的研究工作:
1.在碱性介质中,头孢拉定对鲁米诺-过氧化氢体系的化学发光强度有显著增强作用,据此建立了一种简单、灵敏、稳定的流动注射化学发光测定头孢拉定的新方法。在最佳实验条件下,头孢拉定浓度在1.0×10~(-8) ~ 1.0×10~(-6) g/L内呈良好的线性范围,检出限为6.1×10~(-11) g/L。对质量浓度为1.0×10~(-8) g/L的头孢拉定连续平行测定11次,方法的相对标准偏差(RSD)为1.9%。该方法用于胶囊中头孢拉定含量的测定,回收率在98.8% ~ 103.2%之间。
2.在碱性介质中,氨苄西林钠对鲁米诺-铁氰化钾体系的化学发光有显著增强作用,建立一种流动注射化学发光测定氨苄西林钠的新方法。在优化的条件下,氨苄西林质量浓度的线性范围为5.0×10~(-6) ~ 1.0×10~(-3) g/L,检出限为4.9×10~(-6) g/L。对1.0×10~(-5) g/L的氨苄西林钠连续平行测定11次,方法的相对标准偏差(RSD)为2.1%。该方法用于氨苄西林钠针剂含量的测定,回收率在98.4% ~ 101.2%之间。
3.利用牛血红蛋白(Hb)作为模拟酶催化鲁米诺-过氧化氢体系,头孢哌酮钠对鲁米诺-过氧化氢体系产生的化学发光强度有增强作用,建立了测定头孢哌酮钠的新方法。在最佳条件下,头孢哌酮钠浓度的线性范围为5.0×10~(-6) ~ 1.0×10~(-3) g/L,检出限为2.6×10~(-6) g/L。对4.0×10~(-5) g/L的头孢哌酮钠连续平行测定11次,相对标准偏差(RSD)为1.3%。该方法用于针剂中头孢哌酮钠含量的测定,回收率在97.6% ~ 106.2%。
The process of radiation produced in a chemical reaction from the decay of an excited state to the ground state is known as chemiluminescence (CL). Flow-injection analysis (FIA) is a technology in non-equilibrium thermodynamic conditions which the sample or reagent in the carrier reappearing in the handling zone. Combined with chemiluminescence and flow injection form a new method, it has many features as high sensitivity, wide linear range, quick analysis, simple and easy to implement automation equipment. It has been widely used in biomedicine, environmental monitoring, food hygiene and materials areas. This article is based on the drugs has enhancement or inhibition the luminol system, mainly studies carried out in the following areas:
1.Studied in alkaline medium, cefradine could enhanced the intensity of luminol - H2O2 chemiluminescence system, established a new flow injection chemiluminesce- nce method determination of cefradine with simple, sensitive and stable features. In the optimum conditions, the concentration of cefradine showed good linear relationsh- ip in the range of 1.0×10~(-8) ~ 1.0×10~(-6) g/L with a detection limit of 6.1×10-11 g/L, and the relative standard deviation (RSD) was 1.9% (n=11,ρ=1.0×10~(-8) g/L). This method was applied to determine cefradine in the capsules, and the recoveries were between 98.8% ~ 103.2%.
2.Studied in alkaline medium, ampicillin sodium enhanced luminol-potassium ferricyanide system, established a new flow injection chemiluminescence method to detect ampicillin sodium. In the optimum conditions, the concentration of ampicillin sodium showed good linear relationship in the range of 5.0×10~(-6) ~ 1.0×10~(-3) g/L with a detection limit of 4.9×10~(-6) g/L, and the relative standard deviation (RSD) was 2.1% (n=11,ρ=5.0×10~(-4) g/L). This method was applied to determine ampicillin sodium in the injection, and the recoveries were between 98.4% ~ 101.2%.
3.A novel chemiluminescence method coupled with flow injection technique for the determination of cefoperazone sodium was developed. It was based on the fact that cefoperazone sodium could enhance chemiluminescence intensity when hemoglo- bin was used as a mimetic peroxidase in the catalytic chemiluminescence reaction of luminol and hydrogen peroxidase. In the optimum experimental conditions, the concentration of cefoperazone sodium showed good linear relationship in the range of 5.0×10~(-6) ~ 1.0×10~(-3) g/L with a detection limit of 2.6×10~(-6) g/L, and the relative standard deviation (RSD) was1.3% (n=11,ρ=4.0×10~(-5) g/L). This method was applied to determine cefoperazone sodium in the injection, and the recovery ratio was between 97.6% ~ 106.2%.
1.在碱性介质中,头孢拉定对鲁米诺-过氧化氢体系的化学发光强度有显著增强作用,据此建立了一种简单、灵敏、稳定的流动注射化学发光测定头孢拉定的新方法。在最佳实验条件下,头孢拉定浓度在1.0×10~(-8) ~ 1.0×10~(-6) g/L内呈良好的线性范围,检出限为6.1×10~(-11) g/L。对质量浓度为1.0×10~(-8) g/L的头孢拉定连续平行测定11次,方法的相对标准偏差(RSD)为1.9%。该方法用于胶囊中头孢拉定含量的测定,回收率在98.8% ~ 103.2%之间。
2.在碱性介质中,氨苄西林钠对鲁米诺-铁氰化钾体系的化学发光有显著增强作用,建立一种流动注射化学发光测定氨苄西林钠的新方法。在优化的条件下,氨苄西林质量浓度的线性范围为5.0×10~(-6) ~ 1.0×10~(-3) g/L,检出限为4.9×10~(-6) g/L。对1.0×10~(-5) g/L的氨苄西林钠连续平行测定11次,方法的相对标准偏差(RSD)为2.1%。该方法用于氨苄西林钠针剂含量的测定,回收率在98.4% ~ 101.2%之间。
3.利用牛血红蛋白(Hb)作为模拟酶催化鲁米诺-过氧化氢体系,头孢哌酮钠对鲁米诺-过氧化氢体系产生的化学发光强度有增强作用,建立了测定头孢哌酮钠的新方法。在最佳条件下,头孢哌酮钠浓度的线性范围为5.0×10~(-6) ~ 1.0×10~(-3) g/L,检出限为2.6×10~(-6) g/L。对4.0×10~(-5) g/L的头孢哌酮钠连续平行测定11次,相对标准偏差(RSD)为1.3%。该方法用于针剂中头孢哌酮钠含量的测定,回收率在97.6% ~ 106.2%。
The process of radiation produced in a chemical reaction from the decay of an excited state to the ground state is known as chemiluminescence (CL). Flow-injection analysis (FIA) is a technology in non-equilibrium thermodynamic conditions which the sample or reagent in the carrier reappearing in the handling zone. Combined with chemiluminescence and flow injection form a new method, it has many features as high sensitivity, wide linear range, quick analysis, simple and easy to implement automation equipment. It has been widely used in biomedicine, environmental monitoring, food hygiene and materials areas. This article is based on the drugs has enhancement or inhibition the luminol system, mainly studies carried out in the following areas:
1.Studied in alkaline medium, cefradine could enhanced the intensity of luminol - H2O2 chemiluminescence system, established a new flow injection chemiluminesce- nce method determination of cefradine with simple, sensitive and stable features. In the optimum conditions, the concentration of cefradine showed good linear relationsh- ip in the range of 1.0×10~(-8) ~ 1.0×10~(-6) g/L with a detection limit of 6.1×10-11 g/L, and the relative standard deviation (RSD) was 1.9% (n=11,ρ=1.0×10~(-8) g/L). This method was applied to determine cefradine in the capsules, and the recoveries were between 98.8% ~ 103.2%.
2.Studied in alkaline medium, ampicillin sodium enhanced luminol-potassium ferricyanide system, established a new flow injection chemiluminescence method to detect ampicillin sodium. In the optimum conditions, the concentration of ampicillin sodium showed good linear relationship in the range of 5.0×10~(-6) ~ 1.0×10~(-3) g/L with a detection limit of 4.9×10~(-6) g/L, and the relative standard deviation (RSD) was 2.1% (n=11,ρ=5.0×10~(-4) g/L). This method was applied to determine ampicillin sodium in the injection, and the recoveries were between 98.4% ~ 101.2%.
3.A novel chemiluminescence method coupled with flow injection technique for the determination of cefoperazone sodium was developed. It was based on the fact that cefoperazone sodium could enhance chemiluminescence intensity when hemoglo- bin was used as a mimetic peroxidase in the catalytic chemiluminescence reaction of luminol and hydrogen peroxidase. In the optimum experimental conditions, the concentration of cefoperazone sodium showed good linear relationship in the range of 5.0×10~(-6) ~ 1.0×10~(-3) g/L with a detection limit of 2.6×10~(-6) g/L, and the relative standard deviation (RSD) was1.3% (n=11,ρ=4.0×10~(-5) g/L). This method was applied to determine cefoperazone sodium in the injection, and the recovery ratio was between 97.6% ~ 106.2%.
引文
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