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26044437851
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note
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Trt-S-ON (typically 7 μL of a 0.1 OD per μL, 0.7 OD; 4.16 nmol) was dried in a SpeedVac unit and resuspended in 10 μL of glacial acetic acid. 8.3 μL of a 10 mM solution of 3-nitro-2-pyridinesulfenyl chloride (Cl-NPyS) (8.3 nmol, 20 molar excess) was then added and the reaction was allowed for 1 h. The reaction was monitored by HPLC with a 20 min linear gradient of 12-20% acetonitrile in 50 mM TEAAc, pH 7.2. Prior to HPLC purification, the crude reaction media were resuspended in 500 μL of 50 mM TEAAc and loaded with a manual injector equipped with a 1 mL loop. Analytical HPLC characterization of the activated-ON was performed in the same eluting conditions.
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26044474133
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note
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260nm) were solubilized in 8-10 μL of the matrix 2,4,6-trihydroxyacetophenone (THAP, 45 mg, ammonium citrate, 4 mg) in 500 μL acetonitrile-water (50/50 v/v). The resulting mixture (1 μL) was spotted on the stainless steel probe tip and left to dry in air. The samples were then subjected to MALDI-TOF analysis.
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