Here, a representative synthesis of the UHMW PMMA/[C2mIm][TFSI] gel is described. MMA (0.300 g, 3.00 mmol), [C2mIm][TFSI] (0.700 g, 1.79 mmol), and AIBN (0.1 mg, 0.61 × 10−3 mmol) were charged in a glass vial and sealed with a rubber septum, through which argon was bubbled for 15 min at room temperature. Polymerization was conducted at 80°C for 24 hours. Monomer conversion was determined by 1H-NMR. The molecular weight and polydispersity index of the polymer were determined by GPC using a 10 mM lithium bromide (LiBr)/N,N-dimethylformamide (DMF) solution as the eluent. The GPC system was equipped with a PU-2080 Plus HPLC pump, a DG-2080-53 3-Line degasser, an RI-4030 refractive index detector, a UV-2075 Plus UV/VIS detector, an LC-NetII/ADC interface box, and a CO-4060 column oven (all equipment is manufactured by JASCO, Japan). Two columns (SB-806M HQ, Showa Denko, Japan), which were kept in a column heater at 40°C, were used for separation and calibrated using PMMA standards. For the characterization by 1H-NMR and GPC, the as-prepared UHMW gel pieces were dissolved in CDCl3 (ca. 1 wt %) and 10 mM LiBr/DMF (0.1 wt %) under stirring at room temperature overnight.
Uv 2075 plus uv vis detector
Manufactured by Jasco
Sourced in Japan
The UV-2075 Plus UV/VIS detector is a laboratory instrument designed to measure the absorbance or transmittance of samples in the ultraviolet and visible light spectrum. It is capable of analyzing the light absorption properties of various materials and solutions.
Automatically generated - may contain errors
Lab products found in correlation
Co 4060 column oven, by Jasco (1 mentions)
Dg 2080 53 3 line degasser, by Jasco (1 mentions)
Sb 806m hq, by Resonac (1 mentions)
Pu 2080 plus hplc pump, by Jasco (1 mentions)
Lc netii adc interface box, by Jasco (1 mentions)
Pu 2089 plus hplc pump, by Jasco (1 mentions)
Lc net 2 adc, by Jasco (1 mentions)
Jnm eca600, by JEOL (1 mentions)
Eca 500, by JEOL (1 mentions)
Ecz 400r, by JEOL (1 mentions)
Pu 2080 plus pump, by Jasco (1 mentions)
Rp 18e, by Merck Group (1 mentions)
Hg 980 30, by Jasco (1 mentions)
Borwin software, by Jasco (1 mentions)
Pu 2089 plus quaternary gradient pump, by Jasco (1 mentions)
Lux cellulose 1, by Phenomenex (1 mentions)
4 protocols using uv 2075 plus uv vis detector
1
Synthesis of UHMW PMMA/[C2mIm][TFSI] Gel
2
Analytical Techniques for Organic Synthesis
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All reagents and solvents were
purchased from Tokyo Chemical Industry Co., Ltd.; FUJIFILM Wako Pure
Chemical Corporation; Kanto Chemical Co., Ltd.; Sigma-Aldrich Co.,
LLC; and ISOTEC and used without further purification. Unless otherwise
noted, all reactions were conducted without any inert gas. Chromatography
was carried out with Wakogel C-200 silica gel (FUJIFILM Wako Pure
Chemical Corporation, granule, 0.075–0.150 mm). NMR spectra
were recorded at 600, 500, and 400 MHz for 1H and 150,
125, and 100 MHz for 13C on JEOL JNM-ECA600, -ECA500, and
-ECZ400R spectrometers, respectively. Chemical shifts were reported
in parts per million (ppm, δ) relative to the residual solvent
peaks of CD3OD (3.31 ppm for 1H NMR, 49.0 ppm
for 13C NMR) and (CD3)2CO (2.05 ppm
for 1H NMR, 206.26 ppm for 13C NMR), and coupling
constants (J values) were given in Hertz. High-performance
liquid chromatography was carried out with a PU–2089 plus HPLC
pump (JASCO), an LC–NetII/ADC (JASCO), and a UV–2075
plus UV/vis detector (JASCO). High-resolution mass spectra (HRMS)
were measured on a JEOL Accu TOF T-100 equipped with an electrospray
ionization (ESI) unit.
purchased from Tokyo Chemical Industry Co., Ltd.; FUJIFILM Wako Pure
Chemical Corporation; Kanto Chemical Co., Ltd.; Sigma-Aldrich Co.,
LLC; and ISOTEC and used without further purification. Unless otherwise
noted, all reactions were conducted without any inert gas. Chromatography
was carried out with Wakogel C-200 silica gel (FUJIFILM Wako Pure
Chemical Corporation, granule, 0.075–0.150 mm). NMR spectra
were recorded at 600, 500, and 400 MHz for 1H and 150,
125, and 100 MHz for 13C on JEOL JNM-ECA600, -ECA500, and
-ECZ400R spectrometers, respectively. Chemical shifts were reported
in parts per million (ppm, δ) relative to the residual solvent
peaks of CD3OD (3.31 ppm for 1H NMR, 49.0 ppm
for 13C NMR) and (CD3)2CO (2.05 ppm
for 1H NMR, 206.26 ppm for 13C NMR), and coupling
constants (J values) were given in Hertz. High-performance
liquid chromatography was carried out with a PU–2089 plus HPLC
pump (JASCO), an LC–NetII/ADC (JASCO), and a UV–2075
plus UV/vis detector (JASCO). High-resolution mass spectra (HRMS)
were measured on a JEOL Accu TOF T-100 equipped with an electrospray
ionization (ESI) unit.
3
Quantifying PEA Loading in SLNs via HPLC
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PEA loading level (drug loading, DL), i.e., the percentage amount of PEA in SLNs, was assessed by high performance liquid chromatography (HPLC) analysis. The system consisted of two PU-2080 Plus pumps, an HG-980-30 solvent mixing module, and a UV-2075 Plus UV-Vis detector; data were recorded and processed by Hercule Lite Chromatography Interface and Borwin Software, respectively (Jasco Corporation, Tokyo, Japan). Chromatographic separation was performed using a reversed-phase column (RP-18e, 125 × 4 mm, 5.0 μm) thermostatted at 30 °C and protected by a guard column (4.0 × 4.0 mm, 5.0 μm) (Purospher, Merck, Darmstadt, Germany). The mobile phase consisted of acetonitrile (80%) and water (20%) using an isocratic elution with a flow rate of 1 mL/min. The injection volume was 10.0 µL and the UV detection was carried out at 210 nm. Under these experimental conditions, the retention time of PEA was 8.22 ± 0.90 min.
For the HPLC analysis of PEA loaded in SLNs, 10 mL ethanol was added to 700 µL aliquot of PEA-SLNs suspension, heated at 85 °C for 10 min, and filtered through a 0.2 µm filter (17845Q filters, Sartorius, Goettingen, Germany).
Drug loading (DL) and encapsulation efficiency (EE) values, averaged on three batches of SLNs and labeled SLNs, were calculated by using the following equations:
For the HPLC analysis of PEA loaded in SLNs, 10 mL ethanol was added to 700 µL aliquot of PEA-SLNs suspension, heated at 85 °C for 10 min, and filtered through a 0.2 µm filter (17845Q filters, Sartorius, Goettingen, Germany).
Drug loading (DL) and encapsulation efficiency (EE) values, averaged on three batches of SLNs and labeled SLNs, were calculated by using the following equations:
4
Chiral HPLC Purification of DNA-Copper Complex
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DNA (10 µM) was dissolved in MOPS buffer (1 mL, 20 mM, pH 7.0) containing KCl (150 mM), heated for 3 min at 98 °C, and annealed slowly over the course of 2 h to room temperature. An aqueous solution of copper complex CuL (50 µM) was added and stirred for 30 min at 15 °C. Ten µL of solution 0.5 M of thioanisole in CH3CN, and subsequently 7.5 µL of 3% H2O2 aqueous solution were added. The reaction mixture was stirred for 5 h at 15 °C. At the end of the reaction, diethyl ether (3 mL × 3) was added to extract the products. Anhydrous Na2SO4 was added to the combined organic layers and the solvent was removed under vacuum. The crude products were directly analysed by HPLC using a chiral column. Purification was performed using a Jasco PU-2089 Plus Quaternary Gradient Pump connected to UV-2075 Plus UV/Vis detector (Jasco corporation, Tokyo, Japan) equipped with a Waters Rheodyne injector (Waters Corporation, Milford, MA, USA). HPLC analysis was performed at wavelength 250 nm, using as eluent n-hexane and isopropanol (i-PrOH) 9:1 and a Lux® Cellulose-1 (Phenomenex, 5 μm, 250 mm × 4.6 mm) column.
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