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In April 1572 he was found to be assisting the party of Mary, Queen of Scots who then held Edinburgh Castle, by conveying to The Grange four out of five thousand Crowns which had been sent to her by the Duke of Alva.
In 1567 Serbelloni followed the Spanish armies into Belgium under the Duke of Alva during the repression of the Flemish revolt, being appointed twice as governor of Antwerp.