The Comparison of the Orientation of Sodium 3-Hydroxy-2-Naphthalenecarboxylate in the Cavity of β-Cyclodextrin and Heptakis-(2,3,6-Tri-O-Methyl)-β-Cyclodextrin

Conformational analysis of inclusion complexes of sodium 3-hydroxy-2-naphthalenecarboxylate with 080n5454487v2/xxlarge946.gif" alt="beta" align="MIDDLE" BORDER="0">-cyclodextrin and heptakis-(2,3,6-tri-o-methyl)-080n5454487v2/xxlarge946.gif" alt="beta" align="MIDDLE" BORDER="0">-cyclodextrin in D₂O was investigated by 1D and 2D ¹HNMR measurements. The results show that part of the naphthyl group of sodium 3-hydroxy-2-naphthalenecarboxylate is situated in the 2,3-OH side of the 080n5454487v2/xxlarge946.gif" alt="beta" align="MIDDLE" BORDER="0">-cyclodextrin cavity asymmetrically while the whole naphthyl group is included in the heptakis-(2,3,6-tri-o-methyl)-080n5454487v2/xxlarge946.gif" alt="beta" align="MIDDLE" BORDER="0">-cyclodextrin cavity with the caboxylate and hydroxy group close to the 6-OCH₃ group.     

Study of high-performance liquid chromatographic separation of selected herbicides by hydro-methanolic and micellar liquid chromatography using Genapol X-080 non-ionic surfactant as mobile phase constituent

Chromatographic behaviour of six selected herbicides (chlortoluron, metoxuron, chloridazon, simazine, propazine and atrazine) was studied by reversed-phase (RP) high-performance liquid chromatography (HPLC) containing Genapol X-080 non-ionic surfactant as methanol/water mobile phase constituent. The concentration of methanol was changed from 50 to 0% (v/v) for constant 2% (v/v) concentration of the surfactant. The surfactant concentration in purely aqueous micellar mobile phase varied from 1 to 5% (v/v) what is approximately 360-1800 times above the CMC. Within this concentration range Genapol X-080 proves concentration dependent selectivity changes for chlortoluron/atrazine critical pair not occurred in hydro-methanolic mobile phases. Further studies revealed that this chromatographic system offers high compatibility with cloud-point extraction environmental sample pretreatment approaches using Genapol X-080 for the purpose, too.     

Specific differentiation in Vicia genus by means of capillary electrophoresis

Capillary electrophoresis has been applied to the discrimination of 13 Vicia species, belonging to four sections of Vicia genus. The studied species necessitate of plant growing tests or DNA molecular markers to be distinguished being their seeds morphologically very similar. Alcoholic/saline extracts from dry cotyledons were separated in uncoated fused-silica capillary with iminodiacetic acid isolectric buffer containing hydroxypropylmethylcellulose and acetonitrile. The low intra-specific variation observed for 11 species, suggests that this approach is suitable to carry out species discrimination. Species-specific peaks were identified for V. articulata, V. atropurpurea, V. bithynica, V. benghalensis, V. disperma, V. ervilia, V. monantha, V. sativa and V. villosa. Conversely, V. lutea, V. melanops and V. peregrina, showing very similar electrophoregrams, require other methodological approaches to be discriminated. The discussed CE method appears to have a potential to be regarded as an alternative tool to identify some Vicia species being far less expensive and time consuming than plant growing tests and DNA molecular markers.     

Application of non-ionic surfactant in the microwave-assisted extraction of alkaloids from Rhizoma Coptidis

The feasibility of employing non-ionic surfactant oligoethylene glycol monoalkyl ether (Genapol X-080) as an alternative and effective solvent for the microwave-assisted extraction of alkaloids from Rhizoma Coptidis was demonstrated. When compared with commonly used solvents, 5% Genapol X-080 enhanced the extraction efficiency. Under optimal conditions, i.e. 5% acidified Genapol X-080 (v/v), microwave-assisted extraction for 10 min at 100 °C, the extraction recovery of alkaloids reached 92.8% in a one-step extraction. The efficiency of cloud-point preconcentration of three alkaloids was in the range 93.6-94.7% with relative standard deviation lower than 3.3% by the proposed procedure. Furthermore, the combination of microwave-assisted extraction and cloud-point extraction was shown to be a green, rapid and effective approach for alkaloids preconcentration of Rhizoma Coptidis samples.     

Determination of antihyperglycemic drugs in nanomolar concentration levels by micellar electrokinetic chromatography with non-ionic surfactant

A method for the separation of six selected antihyperglycemic (antidiabetic) drugs (tolbutamide, gliclazide, glimepiride, glibenclamide, repaglinide, and glipizide) was developed with use of micellar electrokinetic chromatography. Two non-ionic poly(ethylene glycol)-based surfactants Genapol X-080 and Triton X-114 (reduced) were studied as neutral pseudostationary phases. High alkaline pH 10.0 was used to obtain negative charges of separated antidiabetic drugs and non-ionic surfactants were employed for selectivity alteration. Both non-ionic surfactants provided good selectivity at concentration 0.2% (v/v) in sodium borate buffer and the separation of six drugs was obtained within 5 min. An on-line preconcentration method based on reversed electrode polarity switching was employed for the determination of antihyperglycemic drugs in blood serum after acetonitrile protein precipitation. The limits of detection ranged from 20.8 nmol L⁻¹ for tolbutamide to 6.5 nmol L⁻¹ for glibenclamide, respectively.