Synthesis · Dual nanozyme based on ultrathin 2D conductive MOF nanosheets intergraded with gold nanoparticles for electrochemical biosensing of H2O2 in cancer cells

5 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs

Metal precursorsHAuCl4.3H2O (500 uL, 0.1 M) added to Cu-HHTP-NS dispersion

Linker precursorsCu-HHTP-NSs preformed from HHTP

SolventsCu-HHTP-NSs dispersion, ethanol and water washes; dry ethanol activation

AtmosphereCapped bottle during heating; activation under vacuum

Temperature65 for Au deposition; 120 for activation

Time0.5 h stirring before heating; 5 h heating; 12 h freeze-drying; 10 h activation

Oxidant / reductantHAuCl4 reduced in situ without added reducing or capping agent

Work-upCentrifugation at 14,000 rpm for 5 min; washed 3 times with ethanol and water; freeze-dried for 12 h.

ActivationImmersed in dry ethanol for 3 days, then heated at 120 deg C under vacuum for 10 h.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	HAuCl4.3H2O	500 uL · 0.1 M	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Other	Cu-HHTP-NSs dispersion	500 mL · 0.1 mg mL-1	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Solvent	ethanol and water	wash amounts not specified	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs

Complete recipeSource: SI

Route 2: Drop Cast

SI text · Preparation of Au-NPs/Cu-HHTP-NSs modified electrode

Solventsisopropanol

AdditivesNafion binder

AtmosphereDried in air; electrochemical tests in N2-saturated PBS

Temperature25 for electrochemical experiments

Substrate orientationPolished 3 mm glassy carbon electrode

Work-upGCE polished with 0.3 and 0.05 um alumina, washed in ethanol and deionised water for 3 min; 5 uL suspension dropped on surface and dried in air.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Au-NPs/Cu-HHTP-NSs nanohybrid	5 mg; 5 uL dropped · 5 mg mL-1 suspension	SI text · Preparation of Au-NPs/Cu-HHTP-NSs modified electrode
Solvent	isopropanol	490 uL	SI text · Preparation of Au-NPs/Cu-HHTP-NSs modified electrode
Additive	Nafion	10 uL	SI text · Preparation of Au-NPs/Cu-HHTP-NSs modified electrode

Partial recipeSource: SI

Route 3: Other

6 · Figure captions · Figure S5

Metal precursorsHAuCl4 (1 mL, 0.1 M)

Linker precursorsCu-HHTP-NSs preformed from HHTP

Oxidant / reductantHAuCl4 reduced in situ; details assumed analogous to main Au-NPs/Cu-HHTP-NSs route

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	HAuCl4	1 mL · 0.1 M	6 · Figure captions · Figure S5
Other	Cu-HHTP-NSs	Not specified	6 · Figure captions · Figure S5

Partial recipeSource: Main

Route 4: Other

2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs

Metal precursorsCu(OAc)2.H2O (same as Cu-HHTP-NSs)

Linker precursorsHHTP (same as Cu-HHTP-NSs)

SolventsWater; methanol wash; dry ethanol activation

AdditivesNaOH; no SDS

AtmosphereNot specified for synthesis; activation under vacuum

TemperatureSame as Cu-HHTP-NSs; 120 during activation

TimeSame as Cu-HHTP-NSs; 10 h activation

Work-upSame procedure as Cu-HHTP-NSs without SDS; activated after synthesis.

ActivationImmersed in dry ethanol for 3 days, then heated at 120 deg C under vacuum for 10 h.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(OAc)2.H2O	same as Cu-HHTP-NSs	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Linker	HHTP	same as Cu-HHTP-NSs	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Base	NaOH	same as Cu-HHTP-NSs	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Solvent	water; methanol; ethanol	same as Cu-HHTP-NSs where applicable	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs

Complete recipeSource: Both

Route 5: Other

2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs

Metal precursorsCu(OAc)2.H2O (560 mg, 2.8 mmol)

Linker precursorsHHTP (600 mg, 1.86 mmol)

SolventsWater (200 mL metal/SDS solution; 400 mL HHTP/NaOH solution); ethanol used for redispersion; methanol wash

AdditivesSodium dodecyl sulfate (SDS, 300 mg, 1.1 mmol); NaOH (300 mg, 7.5 mmol)

AtmosphereNot specified for synthesis; activation under vacuum

Temperature50 during sonication; room temperature overnight; 120 during activation

Time1 h sonication; overnight undisturbed; 12 h settling; 24 h freeze-drying; 10 h activation

Work-upCentrifuged, washed three times with methanol, redispersed in water/ethanol in ultrasonic ice bath for 60 min, settled 12 h, upper colloidal suspension collected, freeze-dried.

ActivationImmersed in dry ethanol for 3 days, then heated at 120 deg C under vacuum for 10 h.

Scalability contextReported Cu-HHTP-NS yield 82.5%; repeated sonication/settling until particles fully exfoliated.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(OAc)2.H2O	560 mg, 2.8 mmol	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Linker	HHTP	600 mg, 1.86 mmol	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Additive	sodium dodecyl sulfate (SDS)	300 mg, 1.1 mmol	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Base	NaOH	300 mg, 7.5 mmol	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Solvent	water	200 mL + 400 mL	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs
Solvent	methanol; ethanol	wash/redispersion amounts not specified	2 · 2.1. Synthesis of Au-NPs/Cu-HHTP-NSs