Volatile organic compounds (VOCs) make up milk flavor and are essential attributes for consumers to evaluate milk quality. In order to investigate the influence of heat treatment on the VOCs of milk, electronic nose (E-nose), electronic tongue (E-tongue) and headspace solid-phase microextraction (HS-SPME)–gas chromatography–mass spectrometry (GC-MS) technology were used to evaluate the changes in VOCs in milk during 65 °C heat treatment and 135 °C heat treatment. The E-nose revealed differences in the overall flavor of milk, and the overall flavor performance of milk after heat treatment at 65 °C for 30 min is similar to that of raw milk, which can maximize the preservation of the original taste of milk. However, both were significantly different to the 135 °C-treated milk. The E-tongue results showed that the different processing techniques significantly affected taste presentation. In terms of taste performance, the sweetness of raw milk was more prominent, the saltiness of milk treated at 65 °C was more prominent, and the bitterness of milk treated at 135 °C was more prominent. The results of HS-SPME-GC-MS showed that a total of 43 VOCs were identified in the three types of milk—5 aldehydes, 8 alcohols, 4 ketones, 3 esters, 13 acids, 8 hydrocarbons, 1 nitrogenous compound, and 1 phenol. The amount of acid compounds was dramatically reduced as the heat treatment temperature rose, while ketones, esters, and hydrocarbons were encouraged to accumulate instead. Furfural, 2-heptanone, 2-undecanone, 2-furanmethanol, pentanoic acid ethyl ester, 5-octanolide, and 4,7-dimethyl-undecane can be used as the characteristic VOCs of milk treated at 135 °C. Our study provides new evidence for differences in VOCs produced during milk processing and insights into quality control during milk production.

Milk titratable acidity is a key indicator of raw milk freshness and quality, but its variation across different dairy animal species remains incompletely characterized. Based on 16,984 raw milk samples from eight dairy animal species (Holstein cow, goat, buffalo, camel, sheep, yak, donkey, and horse) collected within a retrospective raw milk quality monitoring framework in China from 2016 to 2024, this study provides a large-scale descriptive comparison of milk titratable acidity across species. Distinct titratable acidity profiles were observed among species, with camel and yak milk showing relatively high values, sheep, Holstein, and buffalo milk exhibiting intermediate values, and donkey and horse milk presenting markedly low values. Calendar-season-associated patterns also differed among species. Correlations between titratable acidity and milk components varied by species, with relatively stronger positive associations with protein and solids-not-fat (SNF) in several ruminant milks, suggesting that milk composition may contribute to differences in titratable acidity. However, because this study was based on an unbalanced observational dataset with limited animal-level, farm-level, feeding, management, physiological, and environmental metadata, these observations should be interpreted as descriptive and exploratory patterns rather than causal biological mechanisms. This dataset provides preliminary reference information for future studies on species-associated variation in raw milk titratable acidity and for discussions on species-specific raw milk quality evaluation.