Synthesis · Metal-organic framework nanomaterials as novel signal probes for electron transfer mediated ultrasensitive electrochemical immunoassay

6 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

3 · Preparation of Signal-MOFs-Metal Ion Probes

Metal precursorsAu-MOFs

Linker precursorsHKUST-1 in Au-MOFs

SolventsPBS buffer

AdditivesNa2CO3 to pH 9; CRP antibody; BSA

Atmospherenot reported

Temperature4

Timeovernight antibody binding

Work-upPrecipitates washed extensively with water by centrifugation and resuspended in PBS buffer.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Au-MOFs nanoparticles	1 mL aliquot	3 · Preparation of Signal-MOFs-Metal Ion Probes
Solvent	PBS	1 mL	3 · Preparation of Signal-MOFs-Metal Ion Probes
Base	Na2CO3	200 mM	3 · Preparation of Signal-MOFs-Metal Ion Probes
Other	CRP antibody	10 uL · 1 mg/mL	3 · Preparation of Signal-MOFs-Metal Ion Probes
Additive	BSA	25 uL · 1%	3 · Preparation of Signal-MOFs-Metal Ion Probes

Partial recipeSource: Main

Route 2: Other

3 · Preparation of Au-MOFs

Metal precursorsHAuCl4 for citrate Au nanoparticles; cleaned HKUST-1

Linker precursorsHKUST-1 framework

Solventswater; ethanol wash

Atmospherenot reported

Temperatureroom temperature for Au-MOF composite; reflux for Au nanoparticle formation

Time0.1667 reflux after citrate addition for Au NPs; 48 composite reaction

Oxidant / reductanttrisodium citrate solution

Work-upPurple precipitate washed with ethanol and water.

ActivationStored/preserved as washed Au-MOF nanoparticles.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	HAuCl4 solution	50 mL · 0.01%	3 · Preparation of Au-MOFs
Reductant	trisodium citrate solution	2 mL · 1%	3 · Preparation of Au-MOFs
Other	cleaned HKUST-1	50 mg	3 · Preparation of Au-MOFs
Other	gold nanoparticles	15 mL	3 · Preparation of Au-MOFs

Partial recipeSource: Main

Route 3: Solvothermal

2 · Preparation of Pt NPs Modified Covalent Organic Frameworks

Linker precursors0.16 g (15 mmol) 1,4-diaminobenzene; 0.16 g (10 mmol) 1,3,5-triformylbenzene

Solvents10.0 mL 1,4-dioxane; DMF and THF washes; THF Soxhlet extraction

Additives2.0 mL of 3 M acetic acid

Atmospherenot reported

Temperature120; 80 drying

Time72 reaction; 24 Soxhlet; 12 vacuum drying

Work-upYellow solid cooled to room temperature, washed with DMF and THF, isolated by centrifugation, Soxhlet extracted with THF for 24 h.

ActivationDried at 80 C under vacuum for 12 h.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	1,4-diaminobenzene	0.16 g (15 mmol)	2 · Preparation of Pt NPs Modified Covalent Organic Frameworks
Linker	1,3,5-triformylbenzene	0.16 g (10 mmol)	2 · Preparation of Pt NPs Modified Covalent Organic Frameworks
Solvent	1,4-dioxane	10.0 mL	2 · Preparation of Pt NPs Modified Covalent Organic Frameworks
Acid	acetic acid	2.0 mL · 3 M	2 · Preparation of Pt NPs Modified Covalent Organic Frameworks

Vague recipeSource: Main

Route 4: Other

3 · Preparation of MOFs

Metal precursorsCuSO4*7H2O solution

Linker precursors1,3,5-benzenetricarboxylic acid

Solventsmethanol/H2O mixture

Atmospherenot reported

Temperaturenot reported

Time2

Work-upBlue precipitate washed with water by centrifugation until washing solution gave no red precipitate with 6 mol/L HAc and K4[Fe(CN)6].

ActivationResuspended in methanol at 4 C.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*CuSO47H2O solution**	Not specified	3 · Preparation of MOFs
Linker	1,3,5-benzenetricarboxylic acid	Not specified	3 · Preparation of MOFs
Solvent	methanol/H2O mixture	Not specified	3 · Preparation of MOFs

Partial recipeSource: Main

Route 5: Drop Cast

3 · Fabrication of Immunosensor · Scheme 1

Metal precursorsPt-COFs; Au-MOFs-Ab2 signal probe

Linker precursorsCOF framework; HKUST-1 framework

SolventsPBS; aqueous BSA and CRP solutions

Additives0.5% CHIT; anti-CRP; BSA; CRP

Atmospherenot reported

Temperatureroom temperature drying; 4 overnight anti-CRP immobilisation; 37 CRP incubation

Timeovernight anti-CRP immobilisation; 1 BSA blocking; 1 CRP incubation

Substrate orientationglassy carbon electrode

Work-upElectrode washed with distilled water between fabrication steps.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	CHIT	0.5%	3 · Fabrication of Immunosensor · Scheme 1
Other	COFs	1:1 volume ratio with 0.5% CHIT	3 · Fabrication of Immunosensor · Scheme 1
Other	CHIT/COFs solution	10 uL	3 · Fabrication of Immunosensor · Scheme 1
Other	anti-CRP	10 uL · 40 ug/mL	3 · Fabrication of Immunosensor · Scheme 1
Additive	BSA solution	10 uL · 1%	3 · Fabrication of Immunosensor · Scheme 1
Other	CRP	10 uL · different concentrations	3 · Fabrication of Immunosensor · Scheme 1

Partial recipeSource: Main

Route 6: Other

2 · Preparation of Pt NPs Modified Covalent Organic Frameworks

Metal precursors1.0 mL of 1% H2PtCl6

Linker precursorspreformed COFs

Solvents50.0 mL H2O

Atmospherenot reported

Temperature90

Time0.5 ultrasonic dispersion; 12 reflux after sodium citrate addition

Oxidant / reductant3.5 mL of 1% sodium citrate solution

Work-upCentrifuged and washed with water.

ActivationObtained products resuspended in water to preserve.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	COFs	50 mg	2 · Preparation of Pt NPs Modified Covalent Organic Frameworks
Solvent	H2O	50.0 mL	2 · Preparation of Pt NPs Modified Covalent Organic Frameworks
Metal Source	H2PtCl6	1.0 mL · 1%	2 · Preparation of Pt NPs Modified Covalent Organic Frameworks
Reductant	sodium citrate solution	3.5 mL · 1%	2 · Preparation of Pt NPs Modified Covalent Organic Frameworks