Multi-isotope systems have shown great application potential in tracing geological and environmental processes. In order to obtain the isotopic composition of multiple elements of interest, the common protocol is to separate each element from the matrix by independent procedures, which has some limitations, including poor efficiency, being time-consuming, requiring large samples and being unsuitable for rare samples (e.g., meteorite, lunar soil and atmospheric aerosol samples). In this study, we present an integrated and optimized one-step method to separate Cu, Fe, Zn and Cd from complex matrix elements using the AG MP-1M anion exchange resin. By experimentally optimizing the resin volume, eluent concentration and eluent amount, these target elements can be effectively separated from the matrix elements, such as Cu separation from Ti and Co, Zn separation from Fe and Cd, and Cd separation from Sn. The recoveries of Cu, Fe, Zn and Cd were 100.1 ± 0.8% (2SD, n = 3), 99.8 ± 0.7% (2SD, n = 3), 100 ± 0.8% (2SD, n = 3) and 99 ± 1% (2SD, n = 3), respectively. Moreover, the resolution (R) between the elements of interest and interfering elements was in the range of 1.8-28.1. The process blanks of Cu, Fe, Zn and Cd were 1-1.6 ng, 62-70 ng, 2.1-3 ng and 66-74 pg, respectively. The obtained isotope ratios for the standard reference materials agreed well with the published values. Meanwhile, we have reported the Cu, Fe and Zn isotope ratios of six soil and sediment standard reference materials, namely NIST 2711a, GSS-1, GSD-5a, GSD-7a, GSD-12 and GSD-23, for the first time. These new data can be used for the intercalibration and quality control of soils and sediments in other laboratories. The one-step separation of Cu, Fe, Zn and Cd shows obvious economic and efficiency advantages, making it suitable for the simultaneous separation of multiple elements of interest in geological samples.