This dataset contains particulate matter (PM) and organophosphate esters (OPEs) concentration data samples from studies conducted in Limeira - SP, Brazil (22° 33' 43"S e 47° 25' 20"W) between October 2023 and December 2023. In this study, PM was sampled using high-volume air samplers. The instruments collected total suspended particulate matter (TSP) and particles with an aerodynamic diameter less than 10 µm (PM10) through preweighed filters for 24 hours. We also identified six OPEs (TPHP, TDCIPP, TCEP, TNBP, TMPP, and TBOEP) by gas chromatography-mass spectrometry (GC-MS). The spreadsheets contain raw data tabs with mass (g), particle size, date, and weather conditions: temperature (ºC), precipitation (mm), atmospheric pressure (mmHg), and wind (km/h). There are data corresponding to the Zebrafish Embryo Acute Toxicity Test (ZFET) such as survival rate, hatching, and pictures of the tested organisms with the extracted OPEs. In addition, another spreadsheet contains the peak areas for each OPE detected in the extracted PTS and PM10. Analysis conditions are available upon request to the responsible researcher.