Silica silanisation

Dibenzyl-14-crown-4 (lithium ionophore VI 6,6-dibenzyl-l,4,8,ll-tetra-oxa-cyclo-tetradecane) [106868-21-7] M 384.5, m 102-103°. Dissolve in CHCI3, wash with saturated aqueous NaCl, dry with MgSOa, evaporate and purify by chromatography on silica gel and gradient elution with C6Hg-MeOH followed by preparative reverse phase HPLC on an octadecyl silanised silica (ODS) column and eluting with MeOH. It can be crystd from MeOH (v Br 120 cm , C-O-C). [7 Chem Soc Perkin Trans 1 1945 1986.]... 

A commercially packed h.p.l.c. column (25 cm x 4.6 mm) of y-aminopropyl silanised silica [e.g. 5/mi Spherisorb (Regis Chemical Co.), or 7/im Zorbax (Dupont Co.), or 10 /im Lithosorb (Merck), or 5 m irregular (J. T. Baker Chemical Co.)] was sequentially treated, at a pumping rate of 2 ml/min, with the following solutions 2 ml of triethylamine in 40 ml of dry tetrahydrofuran, 2g of (R)-JV-(3,5-dinitrobenzoyl)phenylglycine in 40 ml of dry tetrahydrofuran, 20 ml of dry tetrahydrofuran, and finally 10 per cent propan-2-ol in hexane, until the base line stabilises. The chiral amino acid derivative (which is available from Aldrich Chemical Co.) becomes ionically bonded to the amino residues on the stationary phase. 

Enhancement of a flexible PVC-silica composite interface was studied by the application of gamma-aminopropyltrimethoxysilane on silane. Composites containing silica and silanised silica up to 25.6 phr and prepared by sol-gel technology were subjected to water and water vapour attacks similar to that in their daily use. Silane application resulted in diminishing liquid water and water vapour sorption by about 24.0% and 11.9%, respectively. Inhibition of dioctyl phthalate migration from composites by silane application was also determined as 24% using UV measurements. 20 refs. TURKEY... 

For systems involving the use of aqueous solvents, silanised silicas and hydrophilic polymer based packings with either a polyhydroxyl or polyamide surface are used. 

The main use of TLC in analysis of amoxicillin and its formulated products is as an identity test. A major study [105] using silica gel and silanised silica gel plates with thirty five different mobile phases and iodine vapour detection produced a system, on silanised plates with ammonium acetate/acetone mobile phase, in which amoxicillin was separated from all the other penicillins studied. A slightly modified version of this system was subsequently introduced into the European and British Pharmacopoeia monographs for amoxicillin trihydrate and sodium salt [2]. The British [57,58] and US [9] Pharmacopoeias specify other TLC systems for identification of amoxicillin in formulated products. Simple TLC methods have been developed for identification of several compounds on the WHO essential drugs list, to help combat counterfeiting [106]. For amoxicillin, systems using ethyl acetate/acetic acid/water or acetone/toluene/acetic acid/water with silica gel plates were recommended. 

Nitrogen adsorption/desorption experiments have been performed with silanised silica samples using n-alkyldimethylchlorosilanes with varying chain lengths (Fig. 3.16). 

Fig. 3.16 Nitrogen sorption isotherms at 77 K of silanised silica samples (p/po range from 0.5 to 1).

Table 3.8 Pore structural parameters and ligand densities of silanised silica samples.

The scheme summarises all modern analytical and preparative chromatography protocols, such as high-performance liquid chromatography (HPLC) and gas-liquid chromatography (GLC), with all their conceivable variations. Reverse-phase HPLC or GLC , in which a non-polar liquid is adsorbed onto the solid - the stationary phase - is more appropriate for the analysis of mixtures of derivatives of amino acids and peptides. Cellulose in the above scheme would be replaced by a less-polar medium, such as acetylated cellulose, silanised silica gel, etc. in standard reversed-phase HPLC. 

The MS ion source where electron impact is utilised is maintained at a pressure of <10 r (torr). The sample inlet system is designed to release the analytes into the central region of the source at a carefully controlled rate. This is dependent on the concentration of the analyte and its physical properties. In chromatography interfaces a short length of heated silanised silica or stainless-steel capillary tubing is used to transfer the eluant directly... 

Levarato has developed a series of quantitative methods for the determination of prednisolone along other corticoids after extraction from preparations and separation by TLC on silica gel plates and determination by spectrophotometric (absorption at 240 nm) or colorimetric methods (INH-hydrazone formation, tetrazolium reaction) (81). A simple, fast and quantitative TLC-method for the determination of prednisolone in tablets is described. The method is stability-indicating with respect to accuracy, specificity, sensitivity and precision. The coefficient of variation was between 1.26 and 1.96 % and the sensitivity was about 25 ng. The chromatographic separation was performed on a silicagel plate using two step development of the plate (82). A simple TLC method of separation of prednisolone from other corticosteroids is reported (83). Prednisolone and the dephosphorylated D-homosteroid can be separated on silanised silica gel TLC plates (36). 

Nonionics. The determination of nonionic surfactants using a silanised silica gel GF254 layer with aqueous 80% methanol and the use of a scanning densitometer at 525 nm for detection is described in [43]. Analysis of alkylphenol ethoxylates using a Kieselgel F60 layer with chloroform methanol as mobile phase and IR detection is described in [44]. 

HaO-EtOAc-MeOH 64.3 5.7 30 Silanised silica and triethanol 150d... 

Two of the most useful chiral stationary phases are (8) and (9). Mercaptopropyl silanised silica was alkylated to prepare (8) and this stationary phase permits the resolution of all alkyl 2,4-dinitrophenyl sulphoxides and many 3,5-dinitrobenzoyl derivatives of chiral... 

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