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panyulian0

金虫 (小有名气)

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虫号: 1053857
注册: 2010-07-08
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The starting monomers tetraethoxysilane (TEOS)
99.999%, phenyltrimethoxysilane (PTMOS) 97% and 3-
aminopropyltriethoxysilane (APTES) 99%, 2-ethoxyethanol
99%, HPLC grade acetonitrile (ACN) and sodium hydrogen
phosphate monohydrate (NaH2PO4·H2O), were
purchased from Sigma–Aldrich, Ireland and were used as
supplied. Merck, Sharpe & Dohme Ltd., Clonmel, Ireland,
supplied lisinopril dihydrate. The related substances, d,lhomophenylalanine
(APBA) and para-toluene sulphonic
acid (p-TSA) were purchased from Sigma–Aldrich Ireland.
Three-millilitre SPE reservoirs (75mm × 10 mm, i.d.),
0.20m frits and vac elute system were supplied by JVA
Analytical, Ireland. All of the template solutions used were
prepared in Millipore filtered deionised water.
Polymerisation of varying ratios of the three monomers
above was acid catalysed using concentrated hydrochloric
acid (Fischer Scientific, Ireland Ltd.) in the presence of 2-
ethoxyethanol, which was used as the porogen. After 2 h in
which hydrolysis occurred, the template (0.05 M) was added
producing the imprinted material (MIP). A non-imprinted
polymer (NIP) was prepared in parallel and under identical
conditions with the addition of the template solvent. Condensation
was achieved after 12 h at 80 ◦C. Once synthesised,
the bulk polymers (both MIP and NIP) were finely
ground. Fine particles were removed via a 24-h sedimentation/
filtration process during the extraction process utilising
sonication techniques. After quantitative removal of the template
(95–100%) the ground polymers were packed into SPE
columns. Selectivity was determined by loading of the template
onto the columns and analysing the subsequent extracts
by HPLC.
An isocratic HPLC method (internal communication
2001, Merck Sharpe & Dohme Ltd., Ireland) was used for
quantitative determination of the template using the following
parameters: mobile phase 92%:8%, 0.02M buffer
(pH 5):ACN, flow rate 1 ml/min, column type Zorbax C8
(Carl Stuart Limited, Ireland), 5 m particle size, 250mm × 4.6mm i.d., column temperature 50 ◦C, diode array detector
(DAD) 210 nm. Two-Millilitre sample vials and frits were
purchased from Carl Stuart Ireland Ltd. Analysis of the related
substanceswas carried out using a previously optimised
HPLC method. This method was gradient elution employing
a mixing of the 0.02M sodium hydrogen phosphate buffer
(pH 5) with ACN over a 55-min period. In the initial 35-min
period, the composition changed from 100% to 70% buffer.
This remained constant for a further 10 min at which time the
composition changed back to the original values.

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