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Synthesis of meso-5,10,15,20-Tetrakis(4-N-methylpyridiniumyl)porphyrinato Manganese(III) Pentachloride (Mn−PyP). Mn−PyP was synthesized according to literature methods (Scheme S1, Supporting Information).20 Briefly, porphyrin tetratosylate (101 mg, 0.074 mmol) and manganese(II) chloride tetrahydrate (16 mg, 0.081 mmol) were added to 15 mL of methanol. The mixture was refluxed with stirring under N2 atm. UV−vis absorption spectroscopy was used to monitor the reaction, and it was stopped when the Soret band completely shifted from 422 to 463 nm. Subsequently, the tosylate anion was exchanged by chloride ion on 5 g anion-exchange resin (DOWEX 1 × 8−200) for 24 h with slow stirring. The solution was filtered, and the resin was washed with methanol. The methanol solution was concentrated to 1−2 mL, and the product was precipitated by the addition of Et2O. The precipitate was filtered, washed with Et2O, dried, and dissolved in 4 mL of water. Finally, the manganese salt was allowed to precipitate at 4 °C, and the aqueous phase was filtered and then evaporated. After drying under vacuum, Mn−PyP was obtained as a purple solid. The product was characterized by electrospray ionization mass spectrometry (ESI-MS) (Figure S1). The ESI-MS analysis provided a m/z value of 182.9, whereas the calculated m/z value for [C44H36MnN8]4+ was 182.8, which confirmed the identity and purity of the probe. Assay Procedures. The VEGF luminol CL assay was performed at an ambient temperature. Briefly, 980 μL of Tris− HCl solution (20 mM, pH 9.0) containing 50 nM VEGF165 aptamer 1 (or 80 nM VEGF165 aptamer 2), 10 nM Mn−PyP, 25 μM luminol, 2 mM H2O2, 0.05% Triton X-100, and VEGF of different concentrations were mixed. Then, 20 μL of H 2O2 stock solution (100 mM) was quickly added. The CL signal at 1 min was collected by the MCDR-A system. The photomultiplier tube (PMT) voltage was set at 500 V. The biological fluid analysis was conducted in the sample mixtures containing 0.1%, 1% human serum, or 1% human serum with albumin and IgG removed (Figures S9−S11). The procedures were the same as described above. |
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Cas 72-43-5需要30g，定制合成，能接单的留言
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