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85030272776
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note
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9. Typically; a yohimbine imprinted polymer was made by dissolving yohimbine (0.56 mmol), methacrylic acid (4.6 eq.), ethylene glycol dimethacrylate (35 eq.) and 2,2′-azobis(2,4-dimethylvaleronitrile)(111 mg) in methanol (10 mL), or chloroform (8 mL) containing N,N-dimethylformamide (15% v/v). The solution was cooled on ice and flushed with dry nitrogen after which the polymerization was carried out in a darkened waterbath (45°C) for 18 h. Corynanthine imprinted polymers were prepared as described above, but with the substitution of corynanthine (2) for yohimbine. Blank polymers were prepared as above but in the absence of template. Bulk polymers were ground (2x15min) in a mechanical mortar (Retsch, FRG) and sieved (Retsch, 25 μm) with acetone. Particles of less than 2μm diameter were removed by sedimentation (4x20min) in 200 mL acetone. The polymer particles were washed on a filter funnel, to remove the residual template, with methanol/acetic acid (500 mL, 7:3, v/v), methanol/acetic acid (200 mL, 3:7, v/v) and methanol (200 mL), and were then dried under vaccuum after a final wash with methyl tertbutyl ether (50 mL). All organic solvents and reagents were of analytical or HPLC grade, and the monomer was purified prior to use.
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22
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85030274324
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Polymer combustion analysis data (Mikro Kemi; Uppsala, Sweden): Found: N ≤ 0.02 %
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11. Polymer combustion analysis data (Mikro Kemi; Uppsala, Sweden): Found: N ≤ 0.02 %.
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23
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85030275478
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note
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-1, 75.5 Å.
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24
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85030271078
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note
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-1 (10-14 concentrations per experiment), were mixed in 1 mL acetonitrile/acetic acid, 99.9:0.1 (v/v), and incubated for 20-24 h at room temperature. The polymer particles were separated by centrifugation (11535 x g, 5 min, room temperature) and the radioactivity in 200 μL of the supernatant was measured by liquid scintillation counting (LKB 1219 Rackbeta). 0.5 mg chloroform imprinted polymers or 10 mg methanol imprinted polymers were used in each assay. In the aqueous assays (50mM phosphate buffer pH5.0/Tween20, 99.95:0.05 (v/v)) 10 mg of methanol imprinted polymers per mL buffer were used, and 1.5 mg of chloroform imprinted polymers. Otherwise, analyses were performed as described for the nonaqueous assays.
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14. Nicholls, I. A.; Ramström, O.; Mosbach, K. J. Chromatogr. A 1995, 691, 349-353.
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(1995)
J. Chromatogr. A
, vol.691
, pp. 349-353
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Nicholls, I.A.1
Ramström, O.2
Mosbach, K.3
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