Synthesis · Aggregation-induced enhancement of pyrene-based metal-organic framework as a new electrochemiluminescence emitter for ultrasensitive detection of sulfadimethoxine

7 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

3 · 2.5 Construction of ECL aptasensor · Scheme 1B

Metal precursorsCe-MOF dispersion; AuNPs; ZPM/SP tracer label

Linker precursorsdsDNA from amino-labelled CP and aptamer

SolventsPBS and deionised water washing

Additives6-mercapto-1-hexanol (MCH, 1%); SDM analyte

Atmospherenot reported

Temperature37 for SDM and tracer incubations

Timeovernight dsDNA plus 0.667 h MCH plus 1.5 h SDM plus 2 h tracer

Substrate orientationpolished 4 mm glassy carbon electrode

Oxidant / reductant0.05 M K2S2O8 in PBS for final ECL measurement

Work-upunbound portion gently washed with deionised water after each electrode incubation phase

ActivationGCE polished with 0.3 um and 50 nm Al2O3, sonicated, washed with ethanol and deionised water

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ce-MOF dispersion	10 uL	3 · 2.5 Construction of ECL aptasensor · Scheme 1B
Other	AuNPs	10 uL	3 · 2.5 Construction of ECL aptasensor · Scheme 1B
Other	prepared dsDNA	10 uL	3 · 2.5 Construction of ECL aptasensor · Scheme 1B
Additive	6-mercapto-1-hexanol (MCH)	10 uL · 1%	3 · 2.5 Construction of ECL aptasensor · Scheme 1B
Other	SDM solution	10 uL · various concentrations	3 · 2.5 Construction of ECL aptasensor · Scheme 1B
Other	tracer label	10 uL	3 · 2.5 Construction of ECL aptasensor · Scheme 1B
Electrolyte	PBS	5 mL · 0.1 M, pH 7.0	3 · 2.5 Construction of ECL aptasensor · Scheme 1B
Electrolyte	K2S2O8	0.05 M	3 · 2.5 Construction of ECL aptasensor · Scheme 1B

Complete recipeSource: SI

Route 2: Other

5 · S3 Synthesis of AuNPs

Metal precursorsHAuCl4 (1%, 1 mL)

Solventsdeionised water (100 mL)

AdditivesNa3C6H5O7.2H2O (1%, 2.5 mL)

Atmospherenot reported

Temperatureboiling

Time0.25

Oxidant / reductanttrisodium citrate reductant/stabiliser

Work-upcooled; restored to original volume using deionised water

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	HAuCl4	1 mL · 1%	5 · S3 Synthesis of AuNPs
Solvent	deionised water	100 mL	5 · S3 Synthesis of AuNPs
Reductant	Na3C6H5O7.2H2O	2.5 mL · 1%	5 · S3 Synthesis of AuNPs

Complete recipeSource: Main

Route 3: Other

3 · 2.2 Preparation of Ce-MOF and its dispersion

Metal precursorsCe-MOF powder

Solventsdeionised water

AdditivesPEI (1%, 200 uL)

Atmosphereambient, not otherwise specified

Temperatureroom temperature

Timeovernight

Work-upcentrifuged and washed several times at 10000 rpm for 5 min

Activationsediment re-dispersed in 1 mL deionised water

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ce-MOF	1 mL · 1.2 mg mL-1	3 · 2.2 Preparation of Ce-MOF and its dispersion
Additive	PEI	200 uL · 1%	3 · 2.2 Preparation of Ce-MOF and its dispersion
Solvent	deionised water	1 mL final redispersion	3 · 2.2 Preparation of Ce-MOF and its dispersion

Complete recipeSource: Main

Route 4: Other

3 · 2.2 Preparation of Ce-MOF and its dispersion

Metal precursorsCe(NO3)3.6H2O (108 mg)

Linker precursorstrimesic acid (H3BTC, 52 mg)

Solventsdeionised water (5 mL for solution A); ethanol-H2O (5 mL, v/v = 1:1 for solution B)

Atmospherenot reported

Temperature60

Time1

Work-upwhite precipitate washed three times by centrifugation with deionised water

Activationdried at 60 deg C for 2 h

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ce(NO3)3.6H2O	108 mg	3 · 2.2 Preparation of Ce-MOF and its dispersion
Linker	trimesic acid (H3BTC)	52 mg	3 · 2.2 Preparation of Ce-MOF and its dispersion
Solvent	deionised water	5 mL	3 · 2.2 Preparation of Ce-MOF and its dispersion
Solvent	ethanol-H2O	5 mL · v/v = 1:1	3 · 2.2 Preparation of Ce-MOF and its dispersion

Complete recipeSource: Both

Route 5: Other

3 · 2.4 Formation of dsDNA

Linker precursorsamino-labelled CP (100 uL, 3 uM) and aptamer (100 uL, 3 uM)

Solvents20 mM Tris-HCl buffer (pH 7.4) from SI; oligonucleotide solution buffer contains NaCl, KCl and MgCl2

Atmospherenot reported

Temperature90 then 65 then 25

Time0.25 plus natural cooling

Work-upsolution allowed to cool naturally to 25 C

Activationthermal annealing: 90 C for 5 min, cooled immediately to 65 C and reacted 10 min

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	amino-labelled capture probe (CP)	100 uL · 3 uM	3 · 2.4 Formation of dsDNA
Other	aptamer	100 uL · 3 uM	3 · 2.4 Formation of dsDNA
Solvent	Tris-HCl buffer	20 mM, pH 7.4	3 · 2.4 Formation of dsDNA
Additive	NaCl	140 mM	3 · 2.4 Formation of dsDNA
Additive	KCl	5 mM	3 · 2.4 Formation of dsDNA
Additive	MgCl2	1 mM	3 · 2.4 Formation of dsDNA

Complete recipeSource: Main

Route 6: Solvothermal

3 · 2.1 Synthesis of ZPM

Metal precursorsZn(NO3)2.6H2O (52.36 mg)

Linker precursorsH4TBAPy (41.08 mg)

SolventsDMF (10 mL)

AdditivesHNO3 (240 uL, 65 wt%)

Atmospherenot reported

Temperature120

Time24

Work-upcentrifuged with DMF at 10000 rpm for 5 min; washed several times

Activationdried in vacuum drying oven at 100 deg C

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(NO3)2.6H2O	52.36 mg	3 · 2.1 Synthesis of ZPM
Linker	H4TBAPy	41.08 mg	3 · 2.1 Synthesis of ZPM
Solvent	DMF	10 mL	3 · 2.1 Synthesis of ZPM
Acid	HNO3	240 uL · 65 wt%	3 · 2.1 Synthesis of ZPM

Complete recipeSource: Main

Route 7: Other

3 · 2.3 Preparation of tracer label

Metal precursorsZPM dispersion (1 mg mL-1, 1 mL)

Linker precursorsamino-labelled signal probe (SP, 3 uM, 200 uL)

SolventsMES buffer (1 mL); deionised water redispersion

AdditivesEDC (153.40 mg), NHS (23.02 mg)

Atmospherenot reported

Temperatureroom temperature activation; ice bath coupling

Time12.5

Work-upcentrifuged at 8000 rpm; precipitate re-dispersed in 1 mL deionised water

ActivationEDC/NHS activation of ZPM carboxyl groups for 30 min at room temperature

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	ZPM dispersion	1 mL · 1 mg mL-1	3 · 2.3 Preparation of tracer label
Additive	EDC	153.40 mg	3 · 2.3 Preparation of tracer label
Additive	NHS	23.02 mg	3 · 2.3 Preparation of tracer label
Solvent	MES solution	1 mL	3 · 2.3 Preparation of tracer label
Other	amino-labelled signal probe (SP)	200 uL · 3 uM	3 · 2.3 Preparation of tracer label