Four previously undescribed cyclic peptides, reniochpeptins A-D (1-4), were isolated from the marine sponge Reniochalina sp. Their structures were elucidated through comprehensive spectroscopic analyses and a modified advanced Marfey's method. This method utilized ultra-high-performance liquid chromatography coupled with tandem multiple reaction monitoring mass spectrometry, employing a CORTECS T column to achieve simultaneous separation of derivatized -Leu, -Ile, -allo-Ile, -Leu, -Ile, and -allo-Ile within 25 minutes in a single analytical run.
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