Svancara Ivan, Ogorevc Bozidar, Nović Milko, Vytras Karel
Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, nám. Cs. legií 565, 532 10 Pardubice, Czech Republic.
Anal Bioanal Chem. 2002 Apr;372(7-8):795-800. doi: 10.1007/s00216-002-1263-5. Epub 2002 Apr 4.
A simple and rapid procedure, utilising constant-current stripping analysis (CCSA) at a carbon-paste electrode containing tricresyl phosphate as a pasting liquid (TCP-CPE), has been developed for the determination of iodide in table salt. Because of a synergistic accumulation mechanism based on ion-pairing and extraction of iodide in combination with electrolytic pretreatment of the TCP-CPE, the method is selective for iodide and enables direct determination of iodide in samples of table salt containing anti-caking agents such as K(4)[Fe(CN)(6)] (food additive "E 536") or MgO. The iodide content (calculated as KI) can be determined in a concentration range of 2 to 100 mg kg(-1) salt, with a detection limit (S/N=3) of 1 mg kg(-1), and a recovery from 90 to 115%. The proposed method has been used to determine iodide in several types of artificially iodised table salt and in one sample of natural sea salt. The results obtained agreed well with those obtained by use of three independent reference methods (titration, spectrophotometry, and ICP-MS) used to validate the CCSA method, indicating that the developed method is applicable as a routine procedure for rapid testing in salt production process control and in the analysis of marketed table salts.
已开发出一种简单快速的方法，该方法利用含磷酸三甲苯酯作为糊剂的碳糊电极（TCP-CPE）进行恒电流溶出分析（CCSA）来测定食盐中的碘化物。由于基于离子对和碘化物萃取并结合TCP-CPE的电解预处理的协同富集机制，该方法对碘化物具有选择性，能够直接测定含有抗结剂如K(4)[Fe(CN)(6)]（食品添加剂“E 536”）或MgO的食盐样品中的碘化物。碘化物含量（以KI计算）可在盐浓度范围为2至100 mg kg(-1)内测定，检测限（S/N = 3）为1 mg kg(-1)，回收率为90%至115%。所提出的方法已用于测定几种类型的人工加碘食盐和一个天然海盐样品中的碘化物。获得的结果与使用三种独立参考方法（滴定法、分光光度法和ICP-MS）验证CCSA方法所得到的结果非常吻合，表明所开发的方法适用于作为盐生产过程控制和市售食盐分析中快速检测的常规程序。
