Synthesis · Aptasensor based on gold nanostructure-decorated 2D Cu metal–organic framework nanosheets for highly sensitive and specific electrochemical lipopolysaccharide detection

7 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

3 · Fabrication of electrochemical aptasensors

Linker precursorsThiolated LPS aptamer

SolventsBuffer solutions not fully specified in fabrication paragraph

AdditivesTCEP; 6-mercapto-1-hexanol (MCH); LPS for sensing incubation

AtmosphereNot specified

Temperature37

Time0.667

Substrate orientationAu/Cu-THQ/GCE electrode

Oxidant / reductant1 mM TCEP reduces Apt for 30 min before immobilisation

Work-upIncubate Au/Cu-THQ/GCE with 0.25 uM Apt reduced by 1 mM TCEP for 30 min at 37 C; rinse/dry; incubate with 1 mM MCH for 30 min; rinse; incubate with LPS at 37 C for 40 min; clean before measurements.

Scalability contextSurface functionalisation of individual electrodes.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	LPS aptamer, 5'-HS-(CH2)6-CTTCTGCCCGCCTCCTTCCTAGCCGGATCGCGCTGGCCAGATGATATAAAGGGTCAGCCCCCCAGGAGACGAGATAGGCGGACACT-3'	0.25 uM	3 · Fabrication of electrochemical aptasensors
Reductant	TCEP	1 mM	3 · Fabrication of electrochemical aptasensors
Additive	6-mercapto-1-hexanol	1 mM	3 · Fabrication of electrochemical aptasensors
Other	LPS	various concentrations	3 · Fabrication of electrochemical aptasensors

Complete recipeSource: Both

Route 2: Electrochemical

6 · Electrochemical characterization of Au/2D-MOF/GCE · Figure S5

Metal precursorsHAuCl4 solution (0.1%)

Solvents2D-MOF nanosheet suspension in ethanol; HAuCl4 aqueous solution

AtmosphereDrying with nitrogen steam after GCE cleaning; electrodeposition atmosphere not specified

Temperatureroom temperature drying

Time0.0583

Substrate orientation3 mm diameter polished glassy carbon electrode

Oxidant / reductantElectrodeposition at -0.2 V for 210 s

Work-upGCE polished with 0.3 and 0.05 um alumina, ultrasonically cleaned in water/ethanol/water, dried, drop-cast with 10 uL of 1 mg/mL Cu-TCPP nanosheets, immersed in 0.1% HAuCl4, electrodeposited and dried.

Scalability contextElectrode-scale fabrication only.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-TCPP nanosheets	10 uL · 1 mg/mL	6 · Electrochemical characterization of Au/2D-MOF/GCE · Figure S5
Metal Source	HAuCl4	0.1%	6 · Electrochemical characterization of Au/2D-MOF/GCE · Figure S5
Other	glassy carbon electrode	3 mm diameter	6 · Electrochemical characterization of Au/2D-MOF/GCE · Figure S5

Complete recipeSource: Both

Route 3: Electrochemical

6 · Electrochemical characterization of Au/2D-MOF/GCE · Figure S4

Metal precursorsHAuCl4 solution (0.1%)

Solvents2D-MOF nanosheet suspension in ethanol; HAuCl4 aqueous solution

AtmosphereDrying with nitrogen steam after GCE cleaning; electrodeposition atmosphere not specified

Temperatureroom temperature drying

Time0.0583

Substrate orientation3 mm diameter polished glassy carbon electrode

Oxidant / reductantElectrodeposition at -0.2 V for 210 s

Work-upGCE polished with 0.3 and 0.05 um alumina, ultrasonically cleaned in water/ethanol/water, dried, drop-cast with 8 uL of 1 mg/mL Cu-THQ nanosheets, immersed in 0.1% HAuCl4, electrodeposited and dried.

Scalability contextElectrode-scale fabrication only.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-THQ nanosheets	8 uL · 1 mg/mL	6 · Electrochemical characterization of Au/2D-MOF/GCE · Figure S4
Metal Source	HAuCl4	0.1%	6 · Electrochemical characterization of Au/2D-MOF/GCE · Figure S4
Other	glassy carbon electrode	3 mm diameter	6 · Electrochemical characterization of Au/2D-MOF/GCE · Figure S4

Partial recipeSource: Main

Route 4: Drop Cast

3 · Fabrication of electrochemical aptasensors

Metal precursorsCu-TCPP nanosheets (1 mg/mL suspension)

SolventsEthanolic 2D-MOF nanosheet suspension; ultrapure water/ethanol cleaning solvents

AtmosphereGCE dried with nitrogen steam; final drying at room temperature

Temperatureroom temperature

Substrate orientation3 mm diameter polished glassy carbon electrode

Work-upBare GCE polished with 0.3 and 0.05 um alumina, ultrasonically cleaned in ultrapure water, ethanol and ultrapure water, dried with nitrogen steam, then coated with Cu-TCPP nanosheet suspension and dried.

Scalability contextElectrode-scale drop-cast modification only.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-TCPP nanosheets	suitable volume · 1 mg/mL	3 · Fabrication of electrochemical aptasensors
Other	glassy carbon electrode	3 mm diameter	3 · Fabrication of electrochemical aptasensors
Solvent	ultrapure water and ethanol	used for ultrasonic cleaning	3 · Fabrication of electrochemical aptasensors

Complete recipeSource: Main

Route 5: Solvothermal

3 · Synthesis of Cu-MOF nanosheets

Metal precursorsCu(NO3)2.3H2O (7.2 mg, 0.03 mmol)

Linker precursorsTCPP (8.0 mg, 0.005 mmol)

SolventsDMF/ethanol (v:v = 3:1), 24 mL plus 8 mL linker solution

AdditivesTrifluoroacetic acid (1.6 uL), PVP (20.0 mg)

AtmosphereNot specified

Temperature80

Time3

Work-upSonicated 10 min before heating; washed twice with ethanol; centrifuged at 8000 rpm for 10 min; redispersed in 10 mL ethanol.

Scalability contextSmall-vial nanosheet synthesis; no scale-up data.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.3H2O	7.2 mg, 0.03 mmol	3 · Synthesis of Cu-MOF nanosheets
Linker	TCPP	8.0 mg, 0.005 mmol	3 · Synthesis of Cu-MOF nanosheets
Solvent	DMF and ethanol (v:v = 3:1)	24 mL + 8 mL	3 · Synthesis of Cu-MOF nanosheets
Acid	trifluoroacetic acid	1.6 uL	3 · Synthesis of Cu-MOF nanosheets
Additive	PVP	20.0 mg	3 · Synthesis of Cu-MOF nanosheets

Partial recipeSource: Main

Route 6: Drop Cast

3 · Fabrication of electrochemical aptasensors

Metal precursorsCu-THQ nanosheets (1 mg/mL suspension)

SolventsEthanolic 2D-MOF nanosheet suspension; ultrapure water/ethanol cleaning solvents

AtmosphereGCE dried with nitrogen steam; final drying at room temperature

Temperatureroom temperature

Substrate orientation3 mm diameter polished glassy carbon electrode

Scalability contextElectrode-scale drop-cast modification only.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-THQ nanosheets	suitable volume · 1 mg/mL	3 · Fabrication of electrochemical aptasensors
Other	glassy carbon electrode	3 mm diameter	3 · Fabrication of electrochemical aptasensors
Solvent	ultrapure water and ethanol	used for ultrasonic cleaning	3 · Fabrication of electrochemical aptasensors

Complete recipeSource: Main

Route 7: Other

3 · Synthesis of Cu-MOF nanosheets

Metal precursorsCu(CH3COO)2.H2O (77 mg)

Linker precursorsTetrahydroxy-1,4-benzoquinone hydrate (THQ) (50 mg)

SolventsDegassed H2O, 17 mL for THQ plus 17 mL for Cu/ethylenediamine mixture

AdditivesEthylenediamine (40 uL)

AtmosphereN2 protection

Temperatureroom temperature

Time12

Work-upFiltered; washed twice with H2O (17 mL) and twice with acetone (9 mL); centrifuged at 6000 rpm; dried overnight at 60 C.

Scalability contextAqueous room-temperature batch; no scale-up data.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(CH3COO)2.H2O	77 mg	3 · Synthesis of Cu-MOF nanosheets
Linker	tetrahydroxy-1,4-benzoquinone hydrate (THQ)	50 mg	3 · Synthesis of Cu-MOF nanosheets
Solvent	degassed H2O	34 mL total	3 · Synthesis of Cu-MOF nanosheets
Base	ethylene diamine	40 uL	3 · Synthesis of Cu-MOF nanosheets