At present, liquid phase adsorption
(LPA) is still being quantitatively
characterized in the way of manual sampling and off-line determination
because of the complexity of the system comparing to gas adsorption.
This paper describes a novel method for in situ, real-time measurement
of LPA in general based on fiber-optic sensing (FOS) with the aid
of membranes for the first time. A self-made measurement vessel was
assembled from an adsorption bag, thermostatic devices with a stirrer,
and a fiber-optic dipping probe. Also, macroporous adsorption resins
(MARs) and rutin were chosen as model adsorbent and adsorbate to establish
the FOS system. Here, in situ light absorption measurement was achieved
by eliminating interference of adsorbent particles via encapsulating
them with a membrane into the adsorption bag. In situ LPA measurement
of rutin solution on MARs was obtained by detecting light absorption
at 353 nm using dipping probe, in the broad concentration range from
0.3 to 60 mg/L with excellent linearity (
R
2
= 0.9996). In situ measurements of adsorption and desorption kinetics
on five kinds of MARs with different polarities were systematically
carried out, showing that the adsorption process obeyed the pseudo-second-model.
As well as, the system was proved to be highly accurate and reproducible.
More importantly, this method enabled to study the initial stage of
the adsorption process, starting from the time of the first second,
which is the most important part in the adsorption kinetics, and this
is impossible for traditional sampling methods. The successful application
of FOS to in situ measurement of LPA not only contributes to fast,
automatic, and real-time monitoring of LPA process but also enriches
the research connotation of adsorption.
We describe a stoichiometric approach to the synthesis of molecularly imprinted polymers specific for auramine O. Using the stoichiometric interaction in molecular imprinting, no excess of binding sites is necessary and binding sites are only located inside the imprinted cavities. The free base of the template was obtained to facilitate the interaction with the monomers. Itaconic acid was selected as the functional monomer, and stoichiometric ratio of the interaction with the free base was investigated. The molecularly imprinted polymer preparation conditions such as cross-linker, molar ratio, porogen were optimized as divinylbenzene, 1:2:20 and chloroform/N,Ndimethylformamide, respectively. Under the optimum conditions, a good imprinting effect and very high selectivity were achieved. A solid-phase extraction method was developed using the molecularly imprinted polymers as a sorbent and extraction procedure was optimized. The solid-phase extraction method showed a high extraction recovery for auramine O in its hydrochloride form and free form compared to its analogues. The results strongly indicated that stoichiometric imprinting is an efficient method for development of high selectivity molecularly imprinted polymers for auramine O.
K E Y W O R D Sauramine O hydrochloride, molecularly imprinted polymers, rational design, solid-phase extraction, stoichiometric interactions 1634
Based on the hollow
fiber protected molecularly imprinted polymer,
a micro-solid-phase extraction (μ-SPE) method was developed
and applied for the analysis of indole-3-butyric acid in mung bean
sprouts by high-performance liquid chromatography. The extraction
conditions of the μ-SPE method were optimized using L9(34) orthogonal, and optimum conditions were found as
follows: pH of sample solution was 2.0, chloroform was the organic
solvent for embedding the μ-SPE bars, and acetonitrile was the
desorption solvent. In addition, the extraction time was 80 min, desorption
time was 5 min, stirring speed was 800 rpm, and concentration of NaCl
was 10%. Under the optimum conditions, a standard curve was established
for IBA, with a correlation coefficient of 0.9999. After extraction
with phosphate buffer solution (pH = 9.0), successful pretreatment
of mung bean sprouts was achieved by the μ-SPE method. The limit
of detection was 0.075 mg/kg, and the recoveries were found to be
in the range of 88.9–106.4%. This method is simple, environmentally
friendly, and can be used for the determination of indole auxin contents
in green bean sprouts quickly and accurately.
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