Synthesis evidence

Novel electrochemical sensing strategy for ultrasensitive detection of tetracycline based on porphyrin/metal phthalocyanine-covalent organic framework

Song Y., Meng Y., Chen K. et al. · Bioelectrochemistry · 2024 · 108630

6 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: Main

Route 1: Other

PDF p3 · 2.2. Fabrication of antibiotics aptasensor based on CuTAPc-TFPP-COF

Solventsphosphate buffer / aptamer solution
Additivestetracycline-targeted aptamer
Atmospherenot reported
Temperature4
Time1
Substrate orientationCuTAPc-TFPP-COF/GCE
Work-upCuTAPc-TFPP-COF/GCE incubated in aptamer solution until saturation.
Scalability contextElectrode incubation in 1.5 mL aptamer solution.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
AdditiveTC aptamer, 5'-TCCCTTC CGGTGGTG CTTCCCT-3'1.5 mL · 100 nMPDF p3 · 2.2. Fabrication of antibiotics aptasensor based on CuTAPc-TFPP-COF
Complete recipeSource: SI

Route 2: Electrochemical

PDF p3 · S1.4 Pre-treatment of glassy carbon electrode (GCE)

Solventspiranha solution; ethanol; water; Milli-Q water
Additivesalumina slurry; H2SO4 electrolyte
Atmospheredried under N2 at room temperature
Temperatureroom temperature
Substrate orientation3 mm diameter glassy carbon electrode
Oxidant / reductantpiranha solution H2O2/H2SO4 v:v 3:7; electrochemical activation in 0.5 M H2SO4
Work-upPolished with 0.05 um alumina slurry; washed with piranha solution, ethanol and water for 10 min successively; activated by potential cycling from -0.2 to 1.6 V; rinsed with Milli-Q water.
ActivationElectrochemical activation in 0.5 M H2SO4 from -0.2 to 1.6 V followed by N2 drying.
Scalability contextElectrode pretreatment protocol; no scale-up discussion.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Otherglassy carbon electrodediameter = 3 mmPDF p3 · S1.4 Pre-treatment of glassy carbon electrode (GCE)
Otheralumina slurry0.05 umPDF p3 · S1.4 Pre-treatment of glassy carbon electrode (GCE)
Oxidantpiranha solution (H2O2 and H2SO4)v:v = 3:7PDF p3 · S1.4 Pre-treatment of glassy carbon electrode (GCE)
SolventethanolNot specifiedPDF p3 · S1.4 Pre-treatment of glassy carbon electrode (GCE)
SolventwaterNot specifiedPDF p3 · S1.4 Pre-treatment of glassy carbon electrode (GCE)
ElectrolyteH2SO40.5 MPDF p3 · S1.4 Pre-treatment of glassy carbon electrode (GCE)
SolventMilli-Q waterNot specifiedPDF p3 · S1.4 Pre-treatment of glassy carbon electrode (GCE)
Complete recipeSource: Main

Route 3: Drop Cast

PDF p3 · 2.2. Fabrication of antibiotics aptasensor based on CuTAPc-TFPP-COF

SolventsMilli-Q water
Atmosphereambient drying
Temperatureroom temperature
Time6
Substrate orientationpre-treated glassy carbon electrode
Work-up1.0 mg CuTAPc-TFPP-COF dispersed in 1.0 mL Milli-Q water and ultrasonicated 30 min; about 10 uL dip-coated onto GCE.
ActivationNatural drying for 6 h.
Scalability contextMicrolitre-scale electrode coating.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCuTAPc-TFPP-COF1.0 mg; about 10 uL suspension applied · 1.0 mg mL-1PDF p3 · 2.2. Fabrication of antibiotics aptasensor based on CuTAPc-TFPP-COF
SolventMilli-Q water1.0 mLPDF p3 · 2.2. Fabrication of antibiotics aptasensor based on CuTAPc-TFPP-COF
Complete recipeSource: SI

Route 4: Other

SI text · S1.2 Synthesis of CuTAPc

Metal precursorsCuCl2, 0.6 g
Linker precursors4-nitrophthalonitrile, 1.9 g
SolventsHCl solution; NaOH solution; DMF; Milli-Q water
Additivesurea, ammonium molybdate; Na2S.9H2O reductant
Atmospherenot reported
Temperature160; 90; 60; 70
Time5; 1; 2; 6
Oxidant / reductantNa2S.9H2O used to reduce Cu(II) tetranitrophthalocyanine to CuTAPc
Work-upInitial product stirred in 1 M HCl and NaOH at 90 deg C, cooled, filtered, washed with Milli-Q water; reduction product introduced into water and centrifuged with water until neutral.
ActivationDried in vacuum oven at 60 deg C for 8 h after first stage; final solid dried at 70 deg C for 6 h.
Scalability contextPrecursor synthesis on gram scale for first solid-state stage; no scale-up discussion.
Show 9 structured reagent records
RoleReagentAmount / concentrationSource
Linker4-nitrophthalonitrile1.9 gSI text · S1.2 Synthesis of CuTAPc
Metal SourceCuCl20.6 gSI text · S1.2 Synthesis of CuTAPc
Additiveurea4.8 gSI text · S1.2 Synthesis of CuTAPc
Additiveammonium molybdate100 mgSI text · S1.2 Synthesis of CuTAPc
AcidHCl100 mL · 1 MSI text · S1.2 Synthesis of CuTAPc
BaseNaOH100 mL · 1 MSI text · S1.2 Synthesis of CuTAPc
OtherCu(II) 4,4,4,4-tetranitrophthalocyanine0.75 mgSI text · S1.2 Synthesis of CuTAPc
ReductantNa2S.9H2O2.9 gSI text · S1.2 Synthesis of CuTAPc
SolventDMF30 mLSI text · S1.2 Synthesis of CuTAPc
Partial recipeSource: Main

Route 5: Solvothermal

PDF p3 · 2.1. Synthesis of CuTAPc-TFPP-COF

Metal precursorsCuTAPc metal phthalocyanine building block
Linker precursorsCuTAPc and TFPP
Solventsdimethylformamide (DMF) and o-dichlorobenzene
Additivesglacial acetic acid
Atmospheresealed under vacuum after three freeze-vacuum-thaw cycles in liquid nitrogen
Temperature130
Time72
Work-upCentrifugally washed three times with DMF and methanol, respectively.
ActivationMethanol molecules removed by vacuum drying at 60 deg C for 8 h.
Scalability contextPyrex-tube sealed reaction; quantities and concentrations for CuTAPc, TFPP, solvents and acid are not reported in the supplied main/SI text.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuTAPcnot reportedPDF p3 · 2.1. Synthesis of CuTAPc-TFPP-COF
LinkerTFPPnot reportedPDF p3 · 2.1. Synthesis of CuTAPc-TFPP-COF
Solventdimethylformamide (DMF)not reportedPDF p3 · 2.1. Synthesis of CuTAPc-TFPP-COF
Solvento-dichlorobenzenenot reportedPDF p3 · 2.1. Synthesis of CuTAPc-TFPP-COF
Acidglacial acetic acidnot reportedPDF p3 · 2.1. Synthesis of CuTAPc-TFPP-COF
Complete recipeSource: Main

Route 6: Other

PDF p3 · 2.2. Fabrication of antibiotics aptasensor based on CuTAPc-TFPP-COF

Solventsphosphate buffer / TC solutions
Additivestetracycline analyte
Atmosphereambient electrochemical measurement conditions
Temperatureambient
Substrate orientationApt/CuTAPc-TFPP-COF/GCE
Work-upApt/CuTAPc-TFPP-COF/GCE separately immersed in TC solutions before EIS measurement.
Scalability contextAnalytical incubation state; not a preparative synthesis.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherApt/CuTAPc-TFPP-COF/GCENot specifiedPDF p3 · 2.2. Fabrication of antibiotics aptasensor based on CuTAPc-TFPP-COF
Additivetetracycline (TC)0.1, 1.0, 10, 100, 1000, 10000, and 100000 pMPDF p3 · 2.2. Fabrication of antibiotics aptasensor based on CuTAPc-TFPP-COF