This Data Descriptor presents an anonymized, shuffled dataset of creatinine-normalized urinary metabolite measurements from 73 Bulgarian children with autism spectrum disorder (ASD), released to support reuse in secondary analyses and cross-cohort comparisons. Spot urine results are provided as individual-level values after creatinine normalization; for trimethylamine, values below the limit of quantification (LOQ) were replaced with LOQ/2. The deposit contains measurements for 24 urinary markers grouped into three functional classes (neurotransmitters and aromatic amino acid precursors; one-carbon/methylation and vitamin-related metabolites; and energy metabolism/organic acids with microbiome-related amines). The release includes the results table in both XLSX and CSV formats, a reference limits and units file for contextual interpretation, a data dictionary, a README, a changelog, and SHA-256 checksums for integrity verification. Cohort-level demographics and additional sampling details are described in the companion publication cited in the main text. Dataset: https://doi.org/10.5281/zenodo.18614881 Dataset License: Creative Commons Attribution 4.0 International.