The invention relates to a method for preparing a monolithic stationary phase in the interior volume of a chromatography column made of thermoplastic polymer. This method comprises the following steps: (i) modifying the inner wall of the chromatography column by implementing the following steps: (a) preparing a polymerizable anchoring composition comprising at least one particular methacrylate monomer, one or more solvents and 2,2-dimethoxy-2-phenylacetophenone, (b) depositing, on the inner wall of the column, the polymerizable anchoring composition prepared in step (a), and (c) polymerizing the polymerizable anchoring composition by irradiation with ultraviolet radiation; (ii) introducing, into the interior volume of the column, a polymerizable monolith synthesis composition comprising first and second particular (meth)acrylate monomers, one or more pore-forming agents and a free-radical polymerization initiator; and (iii) polymerizing the polymerizable monolith synthesis composition. The invention also relates to a method for producing a chromatography column comprising such a monolithic stationary phase and to a chromatographic separation method using such a column.

A method of separating a sample is disclosed. The method includes introducing the sample to a fluidic system including a flow path disposed in an interior of the fluidic system, the flow path including an alkylsilyl coating covering wetted surfaces and deposited on the wetted surfaces by thermal decomposing a carbosilane followed by oxidizing the wetted surface, and the alkylsilyl coating is inert to at least one analyte in the sample.

A device for processing samples is disclosed. Interior surfaces of the device, which come in contact with fluids, define wetted surfaces. A portion of the wetted surfaces are coated with an alkylsilyl coating having the Formula I:

##STR00001##

R.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5, and R.sup.6 are each independently selected from (C.sub.1-C.sub.6)alkoxy, NH(C.sub.1-C.sub.6)alkyl, N((C.sub.1-C.sub.6)alkyl).sub.2, OH, OR.sup.A, and halo. R.sup.A represents a point of attachment to the interior surfaces of the fluidic system. At least one of R.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5, and R.sup.6 is OR.sup.A. X is (C.sub.1-C.sub.20)alkyl, O[(CH.sub.2).sub.2O].sub.1-20, (C.sub.1-C.sub.10)[NH(CO)NH(C.sub.1-C.sub.10)].sub.1-20, or (C.sub.1-C.sub.10)[alkylphenyl(C.sub.1-C.sub.10)alkyl].sub.1-20.

The invention provides metal liquid chromatography components with uniformly coated internal surfaces and methods for achieving the same. The invention addresses the problem of corrosion or interference of metal components in the flow path for LC analyses in which the sample interacts with metal ions or surfaces. The invention also alleviates the difficulties in coating very long metal tubes and very small metal channels with an inert, continuous coating that adheres well to metal surfaces. The metal flow path is rendered inert by the coating, and thus compatible with bioanalytical separations, for example, by using a vapor phase deposition process to coat the inner surfaces with a coating that continuously covers all metal surfaces in the flow path.

The present disclosure discusses a method of separating a sample (e.g., pharmaceutical drug, genotoxic impurity, biomarker, and/or biological metabolite) including coating a metallic flow path of a chromatographic system; injecting the sample into the chromatographic system; flowing the sample through the chromatographic system; separating the sample; and analyzing the separated sample using mass spectroscopy. In some examples, the coating applied to the surfaces defining the flow path is non-binding with respect to the sampleand the separated sample. Consequently, the sample does not bind to the low-binding surface of the coating of the flow path. The applied coating can increase the chromatographic peak area for the sample of the chromatographic system.

LC techniques are disclosed. The LC technique includes providing a liquid chromatography system having a coated metallic fluid-contacting element, and transporting a fluid to contact the coated metallic fluid contacting element. Conditions for the transporting of the fluid are selected from the group consisting of the temperature of the fluid being greater than 150 degree Celsius, pressure urging the fluid being greater than 60 MPa, the fluid having a protein-containing analyte incompatible with one of titanium and polyether ether ketone, the fluid having a chelating agent incompatible with the one or both of the titanium or the polyether ether ketone.

Liquid chromatography techniques are disclosed. Specifically, the liquid chromatography technique includes providing a liquid chromatography system having a coated metallic fluid-contacting element, and transporting a fluid to contact the coated metallic fluid-contacting element. Conditions for the transporting of the fluid are selected from the group consisting of the temperature of the fluid being greater than 150? C., pressure urging the fluid being greater than 60 MPa, the fluid having a protein-containing analyte incompatible with one or both of titanium and polyether ether ketone, the fluid having a chelating agent incompatible with the one or both of the titanium or the polyether ether ketone, and combinations thereof.

The present disclosure relates to a chromatographic stationary phase having a uniform polymer density, and related methods. In particular, the present disclosure relates to a method of forming a uniformly dense stationary phase inside a chromatography column.

A method of forming a stationary phase of a capillary column for gas chromatography includes in situ growth of a metal-organic framework on an inner surface of the capillary column. The capillary column may include fused silica on an inner surface thereof and can be treated to provide functional groups capable of forming covalent bonds with a difunctional organic linker of the metal-organic framework. Epitaxial growth of the metal organic framework can occur directly on the inner surface of the capillary tube to a desired uniform thickness, controllable by concentration of metal organic framework precursors.

A device for separating analytes is disclosed. The device has a sample injector, sample injection needle, sample reservoir container in communication with the sample injector, chromatography column downstream of the sample injector, and fluid conduits connecting the sample injector and the column. The interior surfaces of the fluid conduits, sample injector, sample reservoir container, and column form a flow path having wetted surfaces. A portion of the wetted surfaces of the flow path are coated with an alkylsilyl coating that is inert to at least one of the analytes. The alkylsilyl coating has the Formula I:

##STR00001##

R.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5, and R.sup.6 are each independently selected from (C.sub.1-C.sub.6)alkoxy, NH(C.sub.1-C.sub.6)alkyl, N((C.sub.1-C.sub.6)alkyl).sub.2, OH, OR.sup.A, and halo. R.sup.A represents a point of attachment to the interior surfaces of the fluidic system. At least one of R.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5, and R.sup.6 is OR.sup.A. X is (C.sub.1-C.sub.20)alkyl, O[(CH.sub.2).sub.2O].sub.1-20, (C.sub.1-C.sub.10)[NH(CO)NH(C.sub.1-C.sub.10)].sub.1-20-, or (C.sub.1-C.sub.10)[alkylphenyl(C.sub.1-C.sub.10)alkyl].sub.1-20-.