借离子对反相高效液相色谱分离了铱（Ⅳ）和铑（ＩＩＩ） 的２（２咪唑偶氮）苯酚４磺酸（ＩＡＰ４Ｓ）螯合物，并于５６０ ｎｍ 波长处检测之．研究了Ｉｒ（ Ⅳ）和Ｒｈ（ Ⅲ）ＩＡＰ４Ｓ螯合物分离的最宜条件．于Ｎｕｃｌｅｏｓｉｌ Ｃ８ 柱上，用含７．５×１０－３ ｍｏｌ／ＬＫＨ２ＰＯ４Ｎａ２ＨＰＯ４缓冲剂（ｐＨ７．５） 和５．５ ×１０－３ ｍｏｌ／Ｌ溴化四丁基铵的甲醇水（４０：６０，ｖ／ｖ） 作流动相，流速为０．８ ｍＬ／ｍｉｎ． 检测限为１．３ ｎｇ 铱和１．５ ｎｇ 铑． The 2 (2imidazole azo) phenol4sulfonic acid (IAP4S) chelates of iridium (Ⅳ) and rhodium (Ⅲ) were separated by reversed-phase high performance liquid chromatography Wavelength detection. The optimum conditions for the separation of Ir (Ⅳ) and Rh (Ⅲ) IAP4S chelates were studied. Nucleosil C8 column with 7.5 × 10-3 mol / L KH2PO4  Na2HPO4 buffer (pH7.5) and 5.5 × 10-3 mol / L tetrabutylammonium bromide in methanol  water (40 : 60, v / v) as the mobile phase at a flow rate of 0.8 mL / min. The detection limit is 1.3 ng of iridium and 1.5 ng of rhodium.