Synthesis evidence

Novel aptasensing strategy for efficiently quantitative analyzing Staphylococcus aureus based on defective copper-based metal–organic framework

Tian J.-Y., Liu X., Zhang S. et al. · Food Chemistry · 2023 · 134357

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: Drop Cast

SI text · S1.3-S1.6

SolventsMilli-Q water; PBS pH 7.4; ethanol and water for electrode washing; piranha solution for Au electrode pretreatment
AdditivesS. aureus-targeted aptamer solution (100 nM); optional bovine serum albumin (BSA, 0.5%) blocking; alumina slurry (0.05 um) for polishing
AtmosphereDried under N2 during Au electrode pretreatment; otherwise ambient laboratory handling; stored at 4 C when not used.
Temperatureroom temperature
Time1
Substrate orientationpre-treated Au electrode (AE)
Work-upAu electrode polished, rinsed with piranha solution for 5 min, washed with ethanol and water for 5 min, dried under N2, electrochemically activated in 0.5 M H2SO4 from -0.2 to 1.6 V; modified electrodes rinsed with Milli-Q water and PBS after aptamer incubation.
Activation10 mg ML-Cu2O@Cu-MOF dispersed in 10 mL Milli-Q water and ultrasonically agitated for 30 min to form 1 mg/mL suspension before 10 uL drop-casting.
Scalability contextElectrode fabrication uses 10 uL aliquots on Au electrodes.
Show 10 structured reagent records
RoleReagentAmount / concentrationSource
OtherML-Cu2O@Cu-MOF10 mg dispersed in 10 mL; 10 uL drop-cast · 1 mg mL-1SI text · S1.3-S1.6
SolventMilli-Q water10 mL for MOF suspensionSI text · S1.3-S1.6
OtherS. aureus-targeted aptamerincubated for 1 h; sequence reported in SI S1.1 · 100 nM for aptasensor fabrication; stock 1 uMSI text · S1.3-S1.6
Otherbovine serum albumin (BSA)optional blocking step · 0.5%SI text · S1.3-S1.6
OtherAu electrode3 mm diameterSI text · S1.3-S1.6
Otheralumina slurryused for polishing · 0.05 umSI text · S1.3-S1.6
Acidpiranha solution (H2O2 and H2SO4)rinsed for 5 min · H2O2:H2SO4 = 3:7 v/v in S1.3; S1.6 also reports VH2SO4/VH2O2 = 7:3SI text · S1.3-S1.6
AcidH2SO4electrochemical activation from -0.2 V to 1.6 V · 0.5 MSI text · S1.3-S1.6
ElectrolytePBS0.242 g KH2PO4, 1.445 g Na2HPO4*12H2O, 0.2 g KCl, 8.003 g NaCl in 1.0 L Milli-Q water · 0.1 M PBS used for experimentsSI text · S1.3-S1.6
ElectrolyteK3Fe(CN)6/K4Fe(CN)6 in PBS1.65 g K3Fe(CN)6 and 2.111 g K4Fe(CN)6 in 1 L PBS · 5 mM [Fe(CN)6]3-/4- in measurementsSI text · S1.3-S1.6
Partial recipeSource: Both

Route 2: Solvothermal

SI text · S1.2 Synthesis of Cu-BDC, Cu-H3BTC, and Cu-H4EBTC

Metal precursorsCu(NO3)2; amount not explicitly reported for this sole-ligand control in this paper
Linker precursorsH2BDC / BDC sole ligand; paper does not report exact sole-ligand amount
SolventsMain text says similar way to ML-Cu2O@Cu-MOF; exact solvent quantities for this control are not explicitly reproduced
AdditivesPVP-K30 likely by similar route; exact control amount not explicitly reproduced
AtmosphereNot stated; likely sealed autoclave by similar route
Temperature120
Time36
Work-upMain text says prepared by a similar way; exact workup for this control not separately reproduced
ActivationMain text says similar way; exact drying/activation for this control not separately reproduced
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH2BDC / terephthalic acidnot explicitly reported for control synthesis in this paperSI text · S1.2 Synthesis of Cu-BDC, Cu-H3BTC, and Cu-H4EBTC
Metal SourceCu(NO3)2not explicitly reported for control synthesis in this paperSI text · S1.2 Synthesis of Cu-BDC, Cu-H3BTC, and Cu-H4EBTC
Partial recipeSource: Both

Route 3: Solvothermal

SI text · S1.2 Synthesis of Cu-BDC, Cu-H3BTC, and Cu-H4EBTC

Metal precursorsCu(NO3)2; amount not explicitly reported for this sole-ligand control in this paper
Linker precursorsH3BTC sole ligand; paper does not report exact sole-ligand amount
SolventsMain text says similar way to ML-Cu2O@Cu-MOF; exact solvent quantities for this control are not explicitly reproduced
AdditivesPVP-K30 likely by similar route; exact control amount not explicitly reproduced
AtmosphereNot stated; likely sealed autoclave by similar route
Temperature120
Time36
Work-upMain text says prepared by a similar way; exact workup for this control not separately reproduced
ActivationMain text says similar way; exact drying/activation for this control not separately reproduced
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH3BTC / 1,3,5-benzenetricarboxylic acidnot explicitly reported for control synthesis in this paperSI text · S1.2 Synthesis of Cu-BDC, Cu-H3BTC, and Cu-H4EBTC
Metal SourceCu(NO3)2not explicitly reported for control synthesis in this paperSI text · S1.2 Synthesis of Cu-BDC, Cu-H3BTC, and Cu-H4EBTC
Partial recipeSource: Both

Route 4: Solvothermal

SI text · S1.2 Synthesis of Cu-BDC, Cu-H3BTC, and Cu-H4EBTC

Metal precursorsCu(NO3)2; amount not explicitly reported for this sole-ligand control in this paper
Linker precursorsH4EBTC sole ligand; paper does not report exact sole-ligand amount
SolventsMain text says similar way to ML-Cu2O@Cu-MOF; exact solvent quantities for this control are not explicitly reproduced
AdditivesPVP-K30 likely by similar route; exact control amount not explicitly reproduced
AtmosphereNot stated; likely sealed autoclave by similar route
Temperature120
Time36
Work-upMain text says prepared by a similar way; exact workup for this control not separately reproduced
ActivationMain text says similar way; exact drying/activation for this control not separately reproduced
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH4EBTC / diphenylethyne-3,3',5,5'-tetracarboxylic acidnot explicitly reported for control synthesis in this paperSI text · S1.2 Synthesis of Cu-BDC, Cu-H3BTC, and Cu-H4EBTC
Metal SourceCu(NO3)2not explicitly reported for control synthesis in this paperSI text · S1.2 Synthesis of Cu-BDC, Cu-H3BTC, and Cu-H4EBTC
Complete recipeSource: Both

Route 5: Solvothermal

p003 / article p.3 · 2.1. Synthesis of ML-Cu2O@Cu-MOF

Metal precursorsCu(NO3)2 (60 mg, 0.32 mmol)
Linker precursorsH2BDC (16.6 mg), H3BTC (21 mg), H4EBTC (50.6 mg)
Solvents10 mL dichloromethane/methanol, volume ratio 1:1
Additivespolyvinylpyrrolidone-K30 (150 mg)
AtmosphereNot stated; sealed Teflon-lined autoclave.
Temperature120
Time36
Oxidant / reductantNo separate reductant reported; partial Cu2+ reduction to Cu2O inferred during preparation.
Work-upProduct obtained after centrifuging/centrifugalizing and washing.
ActivationDried in vacuum at 60 C for 8 h.
Scalability contextBatch quantities reported at tens to hundreds of milligrams; yield not reported.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)260 mg, 0.32 mmol; purchased from Tianjin Kemiou Chemical Reagent Corporationp003 / article p.3 · 2.1. Synthesis of ML-Cu2O@Cu-MOF
Additivepolyvinylpyrrolidone-K30150 mg; PVP-K30 purchased from Beijing Solarbio Science & Technology Corporationp003 / article p.3 · 2.1. Synthesis of ML-Cu2O@Cu-MOF
Solventdichloromethanepart of 10 mL mixed solvent, 1:1 v/v with methanolp003 / article p.3 · 2.1. Synthesis of ML-Cu2O@Cu-MOF
Solventmethanolpart of 10 mL mixed solvent, 1:1 v/v with dichloromethanep003 / article p.3 · 2.1. Synthesis of ML-Cu2O@Cu-MOF
LinkerH2BDC / terephthalic acid16.6 mg; H2BDC purchased from Aladdin Instrument Corporationp003 / article p.3 · 2.1. Synthesis of ML-Cu2O@Cu-MOF
LinkerH3BTC / 1,3,5-benzenetricarboxylic acid21 mg; H3BTC purchased from Aladdin Instrument Corporationp003 / article p.3 · 2.1. Synthesis of ML-Cu2O@Cu-MOF
LinkerH4EBTC / diphenylethyne-3,3',5,5'-tetracarboxylic acid50.6 mg; H4EBTC supplied by Chemsoon Chemical technology Corporationp003 / article p.3 · 2.1. Synthesis of ML-Cu2O@Cu-MOF