流动注射-化学发光测定香草醛

在酸性条件下,香草醛对Ru(phen)32+-Ce(Ⅳ)反应体系化学发光有显著的减弱作用,据此建立了流动注射-化学发光检测香草醛的新体系。对影响流动注射化学发光的各因素进行了实验研究,优化了反应条件和各项测定参数。结果表明,优化条件下,在质量浓度为4.00×10-7～8.25×10-6g/mL的范围内,相对发光强度与其质量浓度呈对数线性关系,检出限(3σ)为2.90×10-7g/mL,对质量浓度为3.0×10-6g/mL的香草醛进行11次平行测定,相对标准偏差(RSD)为2.6%。对合成样品中香草醛测定的回收率在98.3%～102.8%之间。采样频率120次/h。

Flow-injection chemiluminescence determination of vanillin with the Ru（phen）3～（2+）-Ce（Ⅳ） system

A rapid flow-injection method with chemiluminescence(CL) detection was described for the determination of vanillin in the sulfuric acid medium.It was observed that CL signal of Ru(phen)32+Cerium(Ⅳ) was weakened in the presence of vanillin.The experimental parameters influencing the CL intensity were studied in detail.The analytical approach based on the system was established under the optimal experimental condition.The CL intensity was linear with vanillin concentration in the range of 4.00×10-7～8.25×10-6 g/mL,and the detection limit(3σ) was 2.90×10-7 g/mL.A complete analysis,including sampling and injecting,could be performed in 30 s,giving a through put of about 120/h.The relative standard deviation of 11 determinations was 2.6% for 3.0×10-6 g/mL vanillin.The proposed method was satisfactorily applied to the determination of vanillin in a synthetic sample,the recovery was between 98.3%～102.8%.