Trace metal(loid)s in the environment, such as soil, water, food, and biological samples, are difficult to detect accurately due to their varying concentrations and properties. Understanding their speciation is crucial for evaluating their toxic risk and how they excrete from the human body if overexposure. Knowing the composition and speciation of metal(loid)s can help researchers better assess their health risks. The current collection of research emphasizes some interesting and novel findings using advanced analytical techniques for metal(loid)s. The editors hope it will spark further interest and new studies in this field.