N n dimethylformamide (dmf)

Human serum albumin (HSA, ≥ 98%), Bovine serum albumin (BSA, ≥ 98%), β-Lactoglobulin from bovine blood (β-LG, ≥ 90%), L-Cysteine (Cys, ≥ 98%), IR-780 ( ≥ 98%), and anhydrous dimethyl sulfoxide (DMSO, ≥ 99%) were purchased from Sigma-Aldrich. ICG (modified) for human injection was purchased from Dandong Yichuang Pharmaceutical Co. Ltd. IR-808 ( ≥ 95%) was purchased from Beijing Zhongying Biotechnology Co., Ltd. Cyanine5 NHS ester (Cy5, ≥ 99%) was purchased from Aladdin (Shanghai, China). Recombinant human albumin domain I (DI, ≥ 95%), recombinant human albumin domain II (DII, ≥ 95%), and recombinant human albumin domain III (DIII, ≥ 95%) were purchased from Albumin Therapeutics LLC. Benzo[cd]indol-2(1H)-one, phosphorus pentasulfide, pyridine, sodium hydroxide (NaOH), methyl iodide, acetone, methanol, 2,2-dimethyl-1,3-dioxane-4,6-dione, ethanol, triethylamine, ethyl iodide, N,N-Dimethylformamide (DMF), potassium carbonate, concentrated hydrochloric acid (HCl), potassium iodide, acetic acid, acetic anhydride, 1-iodopropane, 1,4-butylenesulfone, potassium hydroxide, N-methylpyrrolidone(NMP), 2,6-di-tert-butyl-4-methyl pyridine (DTBMP), toluene, 1-butanol, and ethyl 6-bromohexanoate were purchased from Energy Chemical.

All reagents were purchased from commercial sources and used without further purification. 2‐aminoterephthalic acid and pyrimidine‐2,5‐dicarboxylic acid were purchased from Bidepharm. Dried methanol and dried N,N‐dimethylformamide were purchased from Energy Chemical. And, tetrabutyl titanate was purchased from Aladdin. ¹H nuclear magnetic resonance (NMR) spectra were recorded on JNM‐ECZ500R/M1 nuclear magnetic resonance spectrometer (500 MHz). Powder X‐ray diffraction (PXRD) patterns were collected on an X'Pert PRO diffractometer with Cu‐Kα (λ = 1.542 Å) radiation, and scanned at a rate of 5° min⁻¹ in the range of 2–45° (2𝜃) under ambient conditions. Element analysis (EA) was measured by Elementar Unicube elemental analyzer. Scanning electron microscope (SEM) pictures were performed by Hitachi S‐4800 field emission SEM. Thermogravimetric analyses (TGA) were developed on a TA SDT 650 thermal analyzer under nitrogen atmosphere. Differential Scanning Calorimetry (DSC) was performed by Netzsch STA 449F3 simultaneous thermal analyzer.

Tris(4-nitrophenyl)amine (AR, 97%), hydrazine monohydrate (AR, 99%), palladium (10% on carbon; Pd/C), 4′-nitroacetophenone (AR, 98%), thionyl chloride (AR, 98%), 4-aminobenzonitrile (AR, 98%), trifluoromethanesulfonic acid (AR, 98%), 2,3,5,6-tetramethyl-1,4-phenylenediamine (Durene, AR, 98%;), isoquinoline (AR, 97%), and pyridine (AR, 99%) were purchased from TCI Chemical Co., Ltd (Shanghai, China). and used without purification. Pyromellitic dianhydride (PMDA, AR, 97%) and 4,4’-(hexafluoroisopropylidene)-diphthalic andydride (6FDA, AR, 97%) were purchased from Shanghai Aladdin Bio-Chem Technology Co., Ltd. and used after vacuum sublimation. N-methylpyrrolidone (NMP, AR, 99%), 1,3,5-trimethylbenzene (Mesitylene, AR, 99%), and N,N-dimethylformamide (DMF, AR, 99%) were purchased from Energy Chemical Co., Ltd. and used after vacuum distillation. The other analytical grade reagents or solvents were purchased from Energy Chemical Co., Ltd (Shanghai, China). and used as received.

4-Vinylbenzyl chloride (90%), sodium p-styrene sulfonate (SBS), 2,2′-azobis(2-methylpropionitrile) (AIBN), alkynes, N,N-dimethylformamide, and benzenesulfonic acid were supplied by Energy Chemical Company (Shanghai, China). Amberlyst-15 and trifluoromethanesulfonic acid (HOTf) were purchased from Sigma-Aldrich Company (Shanghai, China). Sulfuric acid (98%) was obtained from Tianjin Guangfu Chemical Reagent (Tianjin, China). Tris(4-vinylphenyl)phosphine (TVP) was prepared as our previous report [39 (link)]. 4-Vinylbenzyl-tris-(4-vinylphenyl)-phosphonium chloride (QP) was prepared by a simple reaction of TVP and 4-Vinylbenzyl chloride [40 (link)]. QP, ¹H NMR (400 MHz, CDCl₃): δ = 7.66–7.50 (m, 12H), 7.08–7.02 (m, 4H), 6.69–6.62 (m, 3H), 6.61–6.57 (m, 1H), 5.85 (d, J = 17.6 Hz, 3H), 5.59 (d, J = 17.6 Hz, 1H), 5.43–5.38 (m, 5H), 5.15 (d, J = 10.9 Hz, 1H) ppm.

Benzyl methacrylate (BzMA, 98%, Energy Chemical), ethyl methacrylate (EMA, 99%, Aladdin), 2-hydroxyethyl methacrylate (HEMA, 99%, Aladdin), dimethylacrylamide (DMAA, 98%, Energy Chemical), 1-ethyl-3-methyl imidazolium bis(trifluorosufonylmethane imide) (EMITFSI, 99%, Lanzhou Greenchem), 1-butyl-3-methyl imidazolium hexafluorophosphate (BMIPF₆, 99%, Lanzhou Greenchem), divinylbenzene (DVB, 80%, Energy Chemical), 1-hydroxycyclohexyl phenyl ketone (PI-184, 98%, Aladdin), N,N-dimethylformamide (DMF, 99.9%, Energy Chemical), tetrahydrofuran (THF, 99.9%, Energy Chemical), sodium chloride (NaCl, 99.9%, Energy Chemical), calcium chloride (CaCl₂, 97%, Sigma-Aldrich), magnesium chloride (MgCl₂, 99%, Macklin), potassium chloride (KCl, 99.5%, Energy Chemical), sodium bicarbonate (NaHCO₃, 99.5%, SCR) and magnesium sulfate (MgSO₄, 99.9%, Energy Chemical) were used as received.

Hyaluronic acid (35 kDa) was purchased from Freda Biochem Co., Ltd. (Jinan, Shandong, China). Paclitaxel (PTX) was obtained from Shanghai Zhongxi Sunve Pharmaceutical Co., Ltd. (Shanghai, China). Sorafenib (SOR) was supplied by Meryer Chemical Technology Co., Ltd (Shanghai, China). Soybean phosphatidylcholine was provided by Shanghai Ai Wei Te Pharmaceutical Technology Co., Ltd. Cholesterol was obtained from Beijing J&L Technology Co., Ltd. Deoxycholic acid (DA) was purchased from Shanghai Macklin Biochemical Technology Co., Ltd. Triphosgene, Nε-carbobenzyloxy-L-lysine (Lys), hexylamine, tetrahydrofuran (THF), hexane, N,N-Dimethylformamide (DMF) were obtained from Energy Chemical Technology Co., Ltd (Shanghai, China).