1271-03-0 Purity
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Specification
A method for the preparation of morphologically controllable cross-linked hybrid ferrocenedimethanol derivative cyclophosphazene nanotubes and microspheres is reported. The iron-containing poly(ferrocenedimethanol) cyclotriphosphazene composition was synthesized by a simple polycondensation reaction between 1,1'-ferrocenedimethanol and hexachlorocyclotriphosphazene. The product morphology can be adjusted by introducing two sets of mixed solvent systems.
Synthesis procedures of nanotubes and microspheres
· In a conical flask containing 70 mL of THF and 30 mL of acetonitrile, 1,1'-ferrocenedimethanol (1.32 g) and HCCP (0.35 g) were dissolved. Subsequently, 2 mL of triethylamine was added to the flask. The reaction mixture underwent sonication in an ultrasonic bath (150 W, 40 kHz) for 3 hours at a temperature of 40 °C. The resulting nanotubes were isolated through centrifugation, washed with THF and deionized water, and then dried under vacuum overnight.
· In a conical flask, HCCP (0.35 g) and 1,1'-ferrocenedimethanol (1.32 g) were dissolved in a mixture of 60 mL acetone and toluene (90:10 V:V). Subsequently, 2 mL of triethylamine was added dropwise to the flask after 2 hours. The reaction mixture was ultrasonicated (150 W, 40 kHz) at 40 °C for 3 hours. The microspheres were then separated by centrifugation, washed three times with deionized acetone and water, and dried overnight at 60 °C under vacuum.
A bipodal linker ferrocene derivative (FcD, 1,1'-ferrocenyl bis(methylene lipoate)) was synthesized from 1,1'-ferrocenedimethanol for aggregation of gold nanoparticles (AuNPs). The FcD/AuNP aggregates formed an efficient transduction system for immunosensing based on ferrocene oxidation potential transfer.
Preparation of FcD/AuNP based immunosensor
· First, 1,1'-ferrocenedimethanol (47.2 mg; 0.20 mmol) was combined with 2.2 equivalents of lipoic acid (90.8 mg, 0.44 mmol) in 10 mL of dichloromethane. Following this, 2.2 equivalents of DCC (61.9 mg, 0.3 mmol) and 30% molar of DMAP (7.3 mg, 0.06 mmol) as a catalyst were introduced. The mixture was stirred at room temperature for 24 hours, resulting in a 62% yield of ferrocenyl diester (FcD).
· Next, the freshly synthesized FcD is added to a gold nanoparticle solution in ethanol, resulting in a change in color from red to purple. The pH is adjusted to 9.5 using borate buffer solution.
· The immunosensors are prepared by adding the aHIgG or aGIgG antibody to the FcD/AuNP aggregation and shaking with a mechanical shaker. A BSA solution is then added to block the unconjugated surface of bare gold nanoparticles. The solution is centrifuged, the supernatant is removed, and the solid is dissolved in water.