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作 者:邓光辉[1] 屈忠凯[1] 王士伟[1] 王辉[1] 方梦霞[1] 李训碧
机构地区:[1]广西民族大学化学化工学院,广西林产化学与工程重点实验室,南宁530006
出 处:《分析试验室》2014年第7期819-822,共4页Chinese Journal of Analysis Laboratory
基 金:广西壮族自治区自然科学基金(0640038)资助
摘 要:建立了以三联吡啶钌为发光体系的毛细管电泳电化学发光(CE-ECL)检测系统,并应用于分离和测定西咪替丁片剂中西咪替丁的含量。考察了检测电位,三联吡啶钌(Ru(bpy)3^2+)的溶液浓度,缓冲液的pH和溶液浓度,分离电压、进样电压与进样时间等因素对分离检测的影响。结果表明:在检测电位1.18V,Ru(bpy)3^2+溶液浓度为5 mmol/L,磷酸盐缓冲液(PBS)25 mmol/L(pH 7.8),进样时间10 s,进样电位10 kV,运行电位15 kV下,测得西咪替丁线性范围为2.8×10^-6~4.0×10^-4mol/L,检出限为1.2×10^-7mol/L(S/N=3)。对1.0×10^-5mol/L的西咪替丁标准溶液连续测定5次,电化学发光强度和迁移时间的RSD分别为3.9%和1.5%。方法已应用于西咪替丁片剂中西咪替丁含量的测定。A sensitive and simple method based on capillary electrophoresis(CE) with electrochemiluminescence(ECL) detection has been developed for the separation and determination of cimetidine in cimetidine tablets.The effects of detection potential,the concentration of tris(2,2'-bipyridyl) ruthenium(Ⅱ),the acidity and the concentration of the running buffer,separation voltage,injection voltage,injection time and so on were investigated to acquire the optimum conditions.The detection electrode was a platinum microelectrode with a diameter of 90 μm at a detection potential of 1.18 V(versus Ag/AgCl).Cimetidine could be well separated within 6 min in a 50 cm length fused-silica capillary at a separation voltage of 15 kV in a 25 mmol/L PBS buffer(pH 7.8).The injection voltage and injection time are 10V and 10s.The response was linear over about three orders of magnitude ranging from 2.8 μmol/L to 400 μmol/L for cimetidine.The detection limit(S/N = 3) is 1.2 × 10^-7mol/L.Relative standard deviations(RSD) of no more than 4.0% were obtained for both migration time and electrophoretic peak area.The proposed method was successfully applied to the analysis of active ingredients in cimetidine tablets with satisfactory assay results.
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