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10 protocols using selenium pellets

1

Synthesis and Characterization of Selenium Nanoparticles

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Selenium pellets of about 5 mm, > 99.99% trace metal basis were purchased from Sigma Aldrich, India. The synthesis of the dietary Se was performed in the Nano Lab., School of Applied Science, KIIT University, India using the High Energy Ball Milling (HEBM) through dry milling process according to our previous method [22 (link)]. Characterization of the synthesized Se-Nps was performed using XRD and TEM analysis, in addition to assessing the stability of the particle size distribution of the Se-Nps using a zeta sizer.
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2

Synthesis and Characterization of DNA-Encapsulated Quantum Dots

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The unlabeled and modified, labeled oligonucleotides (HPLC-purified and lyophilized) were obtained from IBA GmbH. N-cyano imidazole (NCI) was synthesized in-house according to previous protocols30 (link). 1-octadecene (ODE, Sigma), oleylamine (Sigma), oleic acid (Sigma), trioctylphosphine (TOP, Cytec), cadmium oxide (Sigma), selenium pellets (Sigma), sulfur powder (Sigma) and tetradecylphosphonic acid (TDPA, PCI synthesis) were purchased from the indicated suppliers. Methods for DNA icosahedron construction and characterization have been previously described30 (link). CdSe/CdS/ZnS QDs were synthesized according to previously published protocols21 (link). The detailed procedures for synthesis, characterization and encapsulation of QDs within DNA icosahedron are provided in the supplementary information. The experiments on cells were carried out using QDs provided by Nexdot (www.nexdot.fr).
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3

Synthesis of Colloidal Semiconductor Nanocrystals

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Oleylamine (OAm, 80–90%), 1-octadecene (ODE, 90%), diphenylphosphine (DPP, 98%), sulfur (S, 99.999%), tris(trimethylsilyl) phosphine (TMS3P, 98%), cadmium oxide (CdO, 99.95%) and hexanes (99%) were purchased from Fisher Scientific. Indium (III) acetate [In(Ac)3, 99.99%], oleic acid (OA, 90%), n-trioctylphosphine (TOP, 97%), selenium pellets (Se, 99.99%), zinc acetate [Zn(Ac)2, 99.0%], dioctylamine (98%), and ethanol (99.8%) were purchased from Sigma-Aldrich. ODE was heated to 120°C under vacuum for several hours prior to use and stored in an argon glovebox. All other chemicals were used directly without further purification. Quartz glass cuvettes were purchased from Starna Cells Inc. All air-sensitive materials were stored and handled in a glovebox under argon.
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4

Synthesis of Colloidal Nanocrystals

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Tri-n-octylphosphine (TOP, 97%), selenium pellets (99.99%), 1 M diethyl zinc solution in hexanes, zinc stearate (ZnSt2, purum, 10–12% Zn basis), hydrogen peroxide solution (H2O2, ≥30%, for trace analysis), and oleylamine (OLA, 70%, tech grade) were purchased from Sigma-Aldrich. 1-Octadecene (ODE, ≥90%, technical grade) was purchased from Alfa Aesar. Anhydrous ethanol, hexanes, and nitric acid (HNO3, trace metal grade) were purchased from Fisher Scientific. Capillary wax and a hot wax pen for sealing quartz capillaries used in SAXS measurements were purchased from Hampton Research. Single-element selenium (10 000 μg/mL in 10% HNO3) and zinc (10 000 μg/mL in 4% HNO3) standard solutions were purchased from High-Purity Standards. (Warning: Et2Zn is pyrophoric, extremely reactive, and should be handled with extreme caution. Appropriate safety practices for the use of oxidizers (H2O2) and strong acids (HNO3) should be observed. The safest order for the combination of HNO3 and H2O2 is the addition of HNO3 to H2O2.)
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5

Synthesis of Colloidal Quantum Dots

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Oleylamine (OAm, technical grade, 70%), 1-octadecene (ODE, 90%), sulfur (S, 99.999%), and hexanes (99%) were purchased from Fisher Scientific. Tris(trimethylsilyl) phosphine ((TMS)3P, 98%) was purchased from Strem Chemical, Inc. Chloroform was purchased from J.T.Baker. Indium (III) acetate (In(Ac)3, 99.99%), oleic acid (OA, 90%), n-trioctylphosphine (TOP, 97%), selenium pellets (Se, 99.99%), zinc acetate (Zn(Ac)2, 99.0%), indium (III) acetylacetonate (In(Acac)3, 99.99%), trioctylphosphine oxide (TOPO, 99%), myristic acid (HMy, 99%), ethanol (99.8%), dioctylamine (97%), and InP/ZnS QDs (λem=670 nm) in toluene were purchased from Sigma-Aldrich. ODE was heated to 120 °C under vacuum for several hours with multiple argon backfill and evacuation cycles to ensure complete removal of air and water and stored in an argon glovebox prior to use. CdSe/ZnS QDs were purchased from NNCrystal US Corporation. All other chemicals were used directly without further purification. Quartz cuvettes were purchased from Starna Cells Inc. All air-sensitive materials were stored and handled in an argon glovebox.
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6

Synthesis and Characterization of Cadmium Chalcogenide Nanocrystals

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All DNA oligonucleotides were purchased from IDT Technologies. Progesterone (PRG), cholesterol (CHL), cortisol (CRT), aldosterone (ALD), estrone (ESN), 5β-pregnane-3ɑ,20-ɑ-diol (PRE), 5β-pregnane-3ɑ,20-ɑ-diol-glucuronide (PRE-Glu), and lysozyme were bought from Sigma Aldrich. Artificial urine DIN EN1616:199 was bought from Pickering Laboratories. RNAprotect Bacteria Reagent was bought from Qiagen. Proteinase K was bought from Roche.
Cadmium oxide (CdO; 99.95%, Alfa Aesar), sulfur (99.95%, ACROS Organics), 1-octadecene (ODE; 90% ACROS Organics), and oleylamine (80–90%) were bought from Fisher Scientific and used as purchased. Zinc acetate (Zn(Ac)2, 99.99%), selenium pellets (Se, 99.99%), trioctylphosphine (TOP, 97%), trioctylphosphine oxide (TOPO, 99%), oleic acid (OA, 90%), poly(isobutylene-alt-maleic anhydride)–6000 g mol−1 (PIMA), (2-aminoethyl)trimethylammonium chloride, histamine, triethylamine, and HEPES (4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid) were obtained from Sigma-Aldrich. HPLC-grade solvents including hexanes (Fisher Scientific), methanol (Honeywell), anhydrous dimethyl sulfoxide (Sigma Aldrich) and chloroform (J.T. Baker) were bought and used without further purification. HEPES 1× is a solution of 25 mM of HEPES and 150 mM of NaCl, adjusted to pH 7.6.
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7

Synthesis of Transition Metal Chalcogenides and Nitrides

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Transition metal chalcogenides were synthesised in a hot-wall quartz tube reactor under low-pressure conditions. The chamber was flushed three times with argon (Ar), and the samples were subsequently heated to 850 °C under 100 sccm Ar. The samples were annealed at this temperature for 30–60 min, and growth was subsequently carried out for 10–15 min by exposing the samples to volatised chalcogen X vapours. The vapours were generated by heating solid chalcogen precursors situated upstream from the samples: ~110 °C for sulphur (sulphur flakes; Sigma Aldrich), ~220 °C for selenium (selenium pellets; Sigma Aldrich), and ~420 °C for tellurium (tellurium pieces; Sigma Aldrich). After growth, the samples were naturally cooled to room temperature under 100 sccm Ar flow. Synthesis of continuous MoS2 films for electrical device measurements was achieved by increasing the growth temperature to 950 °C.
Identical processing conditions were used to synthesise transition metal nitrides in a cold-wall reactor (AIXTRON Black Magic), except that the entire process was done under 100 sccm H2 flow instead of argon in order to mitigate surface oxidation of the alloys. The growth of nitrides was performed by introducing 5 sccm NH3 into the chamber for 5 min The samples were then naturally cooled down to room temperature under 100 sccm H2.
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8

Selenium Pellet Synthesis and Characterization

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Selenium pellets (Se, diameter <5 mm, purity ≥99.99% based on trace metals analysis) and sodium hydroxide (NaOH, American Chemical Society reagent, ≥97.0%, pellets) were purchased from Sigma-Aldrich (St Louis, MO, USA).
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9

Synthesis of Colloidal Semiconductor Nanocrystals

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All reagents were used as purchased from the
manufacturer without further purification. The following were purchased
from Sigma-Aldrich: trioctylephosphine (TOP; cat: 718165), selenium
pellets (Se; cat: 209643), diphenylphosphine (DPP; cat: 252964), cadmium
oxide (CdO; cat: 202894), trioctylphosphine oxide (TOPO; cat: 223301),
1-hexadecylamine (HDA; cat: 445312), tetradecylphosphonic acid (TDPA;
cat: 736414).
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10

Synthesis and Characterization of DNA-Encapsulated Quantum Dots

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The unlabeled and modified, labeled oligonucleotides (HPLC-purified and lyophilized) were obtained from IBA GmbH. N-cyano imidazole (NCI) was synthesized in-house according to previous protocols30 (link). 1-octadecene (ODE, Sigma), oleylamine (Sigma), oleic acid (Sigma), trioctylphosphine (TOP, Cytec), cadmium oxide (Sigma), selenium pellets (Sigma), sulfur powder (Sigma) and tetradecylphosphonic acid (TDPA, PCI synthesis) were purchased from the indicated suppliers. Methods for DNA icosahedron construction and characterization have been previously described30 (link). CdSe/CdS/ZnS QDs were synthesized according to previously published protocols21 (link). The detailed procedures for synthesis, characterization and encapsulation of QDs within DNA icosahedron are provided in the supplementary information. The experiments on cells were carried out using QDs provided by Nexdot (www.nexdot.fr).
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