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The present work evaluated a microwave-assisted wet digestion method using diluted HNO
with in situ UV radiation for the digestion of starch and skimmed milk powder for further metals determination by spectrometric plasma-based techniques. The sample digestion was conducted using an in situ UV lamp (electrodeless discharge lamp), and the digestion efficiency was improved by employing O
(20 bar) and 2 mL 30 % H
O
as auxiliary reagents. The accuracy of the proposed digestion method was evaluated by metals determination (Ca, Cd, Cu, Fe, K, Mg, Mo, Mn, Na, Pb, and Zn) in certificated reference material, which agreed with certified values (Student t-test <0,05). With the use of a UV lamp an environmentally friendly protocol was developed for starch and skimmed milk powder digestion using 0.1 mol L
HNO
with auxiliary reagents (H
O
or O
). The RCC value ranged from 0.9 to 1.2 % (starch and skimmed milk powder, respectively). The simultaneous cooling approach further improved the digestion efficiency (RCC <0,3 % for both samples), allowing to use milder digestion conditions, or even just water, being environmentally friendly, reducing the waste generation and reagents consumption, allowing food quality control through a greener approach.