Corbo Dennys, Bertotti Mauro
UNIb, Universidade Ibirapuera, São Paulo, SP, Brazil.
Anal Bioanal Chem. 2002 Oct;374(3):416-20. doi: 10.1007/s00216-002-1504-7. Epub 2002 Sep 11.
A flow injection analysis (FIA) method has been developed for the determination of sulphite in beverages. The method is based on the amperometric detection (0.60 V vs Ag/AgCl (sat. NaCl)) of the analyte at a copper surface in an alkaline medium (1 M NaOH solution) with a manifold that incorporates flow extraction of sulphite as SO2 through a PTFE membrane. Under optimal experimental conditions the peak current response increases linearly with sulphite concentration over the range from 1.0 to 5.0 mM. The repeatability of the electrode response in the FIA configuration was evaluated as 4% ( n =20), the limit of detection of the method was 0.04 mM (S/N =3) and the analytical frequency was 50 h(-1). Since ethanol is also electroactive and permeates through the PTFE membrane, a strategy involving in a first step measurements of only ethanol by manipulating the pH of the donor stream was employed for wine samples. Then, both ethanol and sulphite were measured at the copper electrode at 0.40 V vs Ag/AgCl (sat. NaCl) and the sulphite concentration was determined by difference. Results for 3 different beverage samples (alcoholic and non-alcoholic) showed excellent agreement with the ones obtained by using a recommended procedure for sulphite analysis.
已开发出一种流动注射分析(FIA)方法用于测定饮料中的亚硫酸盐。该方法基于在碱性介质(1 M NaOH溶液)中,在铜表面对分析物进行安培检测(相对于Ag/AgCl(饱和NaCl)为0.60 V),其流路包含通过聚四氟乙烯膜以SO₂形式对亚硫酸盐进行流动萃取。在最佳实验条件下,峰电流响应在1.0至5.0 mM范围内随亚硫酸盐浓度呈线性增加。在FIA配置中电极响应的重复性评估为4%(n = 20),该方法的检测限为0.04 mM(S/N = 3),分析频率为50 h⁻¹。由于乙醇也具有电活性且能透过聚四氟乙烯膜,对于葡萄酒样品采用了一种策略,即第一步通过控制供液流的pH仅测量乙醇。然后,在相对于Ag/AgCl(饱和NaCl)为0.40 V的铜电极上同时测量乙醇和亚硫酸盐,并通过差值确定亚硫酸盐浓度。3种不同饮料样品(含酒精和不含酒精)的结果与使用推荐的亚硫酸盐分析方法获得的结果高度一致。