Black tea's quality and flavor are largely influenced by its processing stages, which affect its volatile and non-volatile phytochemicals. This study aimed to optimized black tea manufacturing by investigating withering time, fermentation time, and temperature's impact on sensory quality. Using a U*15 (157) uniform design, optimal conditions were determined: 14 h of withering, 5.6 h of fermentation, and a 34 °C temperature. A verification experiment analyzed the volatile and non-volatile profiles. HPLC, GC–MS, and LC-MS revealed dynamic changes in phytochemicals. Among 157 VOCs and 2642 metabolites, 19 VOCs (VIP > 1.5) were crucial for aroma, while 50 (VIP > 1.5, p < 0.01) characteristic metabolites were identified. During processing, fragrant volatile compounds like linalool oxides, geraniol, benzeneacetaldehyde, benzaldehyde, methyl salicylate, and linalyl acetate increased, contributing to rose and honey like aromas. These changes were crucial in developing the characteristic flavor and color of black tea. Twenty-four new compounds formed, while 80 grassy odor volatiles decreased. Non-volatile metabolites changed notably, with decreased catechins and increased gallic acid. Theaflavin compounds rose initially but declined later. This study outlines metabolite changes in Yunkang 10 black tea, crucial for flavor enhancement and quality control.
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