Synthesis · Rapid and sensitive detection of PD-L1 exosomes using Cu-TCPP 2D MOF as a SPR sensitizer

4 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Electrochemical

3 · 2.4. Construction and characterization of SPR sensor chip for detection of PD-L1 exosomes

Metal precursorspreformed Cu-TCPP 2D MOF nanosheet solution; gold electrode substrate

Solventsethanol and deionized water during sonication/rinsing; 0.5 M H2SO4 for electrochemical activation

Additivesalumina polishing suspensions (0.3 um, 0.05 um)

Atmospherenitrogen drying; ambient atmosphere otherwise not reported

Temperatureroom temperature

Substrate orientationpolished gold electrode surface

Oxidant / reductantpiranha solution 98% H2SO4:30% H2O2 = 3:1 for 5 min pretreatment

Work-upPolish with alumina, sonicate in ethanol and deionized water, piranha clean, rinse, electrochemically activate in 0.5 M H2SO4, dry with nitrogen, then apply the same modification steps as SPR sensors.

Activationelectrochemical activation in 0.5 M H2SO4

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	gold electrode	Not specified	3 · 2.4. Construction and characterization of SPR sensor chip for detection of PD-L1 exosomes
Other	alumina polishing solution	0.3 um, 0.05 um	3 · 2.4. Construction and characterization of SPR sensor chip for detection of PD-L1 exosomes
Solvent	ethanol	Not specified	3 · 2.4. Construction and characterization of SPR sensor chip for detection of PD-L1 exosomes
Solvent	deionized water	Not specified	3 · 2.4. Construction and characterization of SPR sensor chip for detection of PD-L1 exosomes
Acid	H2SO4	98% in piranha; 0.5 M for activation	3 · 2.4. Construction and characterization of SPR sensor chip for detection of PD-L1 exosomes
Oxidant	H2O2	30% in piranha	3 · 2.4. Construction and characterization of SPR sensor chip for detection of PD-L1 exosomes
Other	2D MOF nanosheet solution	same modification steps as SPR sensors; concentration not restated for GE	3 · 2.4. Construction and characterization of SPR sensor chip for detection of PD-L1 exosomes

Complete recipeSource: Main

Route 2: Other

3 · 2.4. Construction and characterization

Metal precursorspreformed 2D MOF-chip

Solventsdeionized water buffer baseline

Additivesmultifunctional peptide SS-IMVTESSDYSSY-KK-FHYQRDTPKSYN

Atmospherenot reported

Temperatureroom temperature

Substrate orientation2D MOF-modified gold SPR chip

Work-up300 uL peptide solution flowed at 5 uL/min; PD-L1 exosomes subsequently flowed at 5 uL/min.

Activationpi-pi stacking of peptide on Cu-TCPP MOF surface

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	SS-IMVTESSDYSSY-KK-FHYQRDTPKSYN peptide	300 uL · 100 ug/mL	3 · 2.4. Construction and characterization
Other	PD-L1 exosomes	300 uL · different concentrations	3 · 2.4. Construction and characterization

Complete recipeSource: Main

Route 3: Drop Cast

3 · 2.4. Construction and characterization

Metal precursorspreformed Cu-TCPP 2D MOF nanosheet solution

Solventsethanol and deionized water rinse; MOF stored/deposited from ethanol solution

Atmospherenitrogen drying; deposition atmosphere not reported

Temperatureroom temperature

Time0.5

Substrate orientationtreated SPR gold chip surface

Oxidant / reductantmild piranha solution H2SO4:30%H2O2 = 3:1 for 40 s pretreatment

Work-upRinse with deionized water to remove excess MOF; dry with nitrogen; fix in SPR instrument.

Activationgold chip cleaning in ethanol/deionized water and mild piranha solution

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	2D MOF nanosheet solution	50 uL · appropriate concentration; optimized at 10 ug/mL	3 · 2.4. Construction and characterization
Acid	H2SO4	mild piranha H2SO4:30%H2O2 = 3:1	3 · 2.4. Construction and characterization
Oxidant	H2O2	30%	3 · 2.4. Construction and characterization

Complete recipeSource: Main

Route 4: Hydrothermal

3 · 2.3. Synthesis of Cu-TCPP 2D MOF

Metal precursorsCu(NO3)2.3H2O (3.6 mg, 0.015 mmol)

Linker precursorsTCPP (4.0 mg, 0.005 mmol)

SolventsDMF/ethanol, V:V = 3:1; 12 mL for metal/PVP/TFA solution plus 4 mL for TCPP solution

Additivestrifluoroacetic acid (1.0 M x 10 uL); PVP (10.0 mg)

Atmospherenot reported

Temperature80

Time3

Work-upCool to room temperature; centrifuge at 8000 rpm for 10 min; wash twice with ethanol; redissolve in 10 mL ethanol; store at 4 C.

Activationnone reported

Scalability contextPaper describes the method as simple and rapid; no yield or scale-up study reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.3H2O	3.6 mg, 0.015 mmol	3 · 2.3. Synthesis of Cu-TCPP 2D MOF
Linker	TCPP	4.0 mg, 0.005 mmol	3 · 2.3. Synthesis of Cu-TCPP 2D MOF
Solvent	N,N-dimethylformamide (DMF) and ethanol	12 mL plus 4 mL mixed solvent · V:V = 3:1	3 · 2.3. Synthesis of Cu-TCPP 2D MOF
Acid	trifluoroacetic acid	10 uL · 1.0 M	3 · 2.3. Synthesis of Cu-TCPP 2D MOF
Additive	PVP	10.0 mg	3 · 2.3. Synthesis of Cu-TCPP 2D MOF