流动注射-化学发光法测定苯磺酸氨氯地平
FI-Chemiluminescence Determination of Amlodipine Besylate
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摘要: 报道了基于铁氰化钾与鲁米诺化学反应,并应用IFFM-E型流动注射化学发光分析仪测定苯磺酸氨氯地平(ALDP)的方法。在碱性溶液中,上述化学发光反应的化学发光强度因ALDP的存在而显著增加,且其强度的增加值(ΔI)与ALDP的质量浓度分别在以下3个浓度区间呈线性关系:3.0×10-6~8.0×10-5g·L-1,8.0×10-5~7.0×10-4g·L-1及7.0×10-4~5.0×10-3g·L-1。方法的检出限(3σ)为8.5×10-7g·L-1。分析时取ALDP药片10片研碎为粉末状,称取其总质量的1/10溶于水中,定容至50 mL,分取适量并稀释后供分析用。试样的进样体积为150 μL,引入仪器的铁氰化钾溶液、氢氧化钠溶液及鲁米诺溶液的浓度依次为2.0×10-4,5.0×10-2,2.0×10-5mol·L-1。在已知ALDP含量的试样溶液中分别加入3个不同浓度的ALDP标准溶液,按方法测定后求得其回收率在96.0%~102.4%之间。对为5.0×10-4g·L-1 ALDP标准溶液重复测定11次,所得相对标准偏差为1.7%。Abstract: FI-chemiluminescence (using the IFFM-E FI-CL analyzer) determination of Amlodipine besylate (abbreviated as ALDP) based on the CL reaction between K3Fe(CN)6 and luminol was reported. In an alkaline solution, the CL intensity of the CL reaction was remarkably enhanced by the presence of ALDP, and linear relationship between values of increase in CL intensity (ΔI) and mass concentration of ALDP was obtained in 3 sectional ranges of 3.0×10-6-8.0×10-5g·L-1, 8.0×10-5-7.0×10-4g·L-1 and 7.0×10-4-5.0×10-3g·L-1. Detection limits (3σ) was found to be 8.5×10-7g·L-1. Ten tablets of ALDP were taken and ground to powder and 1/10 of the total mass of the powdered sample was dissolved in water and made up to a volume of 50 mL. An aliquot of suitable concentration was taken for analysis. Volume of sample introduction taken was 150 μL. Concentrations of the solutions of K3Fe(CN)6, NaOH and luminol taken for the FI-CL analysis were 2.0×10-4, 5.0×10-2 and 2.0×10-5mol·L-1 respectively. Recovery was tested by addition of ALDP standard solutions of different concentrations to sample solutions of known ALDP concentrations, values of recovery obtained were in the range of 96.0%-102.4%. Value of RSD (n=11) obtained from determination of ALDP at a concentration of 5.0×10-4g·L-1 was 1.7%.