Publication detail

High pressure modification of the simple automated liquid chromatographic system for splitless nano column gradient separations

ŠESTÁK, J. KAHLE, V.

Original Title

Type

journal article - other

Language

English

Original Abstract

In this work we have modified our concept of simple splitless gradient liquid chromatographic system for micro and nano columns with backpressure up to 50 bar. Presented configuration allows us to run analysis under the pressure up to 400 bar. Experimental configuration consists of an OEM programmable syringe pump equipped with a 250-ul high-pressure syringe and ten-port selector valve. High pressure syringe is connected to central port of selector valve via 0.5 meter long PEEK capillary of 380 um i. d. fixed in horizontal plane. PEEK capillary here serves as gradient generator as well as gradient loop and as sample loop. Mobile phase gradients are created by successive sucking of defined volumes of four water-acetonitrile solutions with gradually changing acetonitrile concentration into the PEEK capillary. Sharp mobile phase boundaries fade out while passing through the valve body and due to the parabolic profile of laminar flow as well as due to diffusion. Available linear gradients of volumes from 5 to 50 ul traced by uracil are presented. Sample introduction is performed as separate step. Before preparing gradient, relatively large volume of sample is sucked into the PEEK capillary. Desired volume of sample is then injected on the column and excessive volume is drained. Major advantage of this approach is the fact that real large volume of sample (tens of microliters) could be injected and pre-concentrated on-column. Another benefit of presented design is that reversed mobile phase gradients for column regeneration or for HILIC separation mode are available without any change of system arrangement. System performance was evaluated and good values of relative standard deviation of retention times and sample injection volumes were received.

Keywords

nanocolumn liquid chromatography; splitless gradient

Authors

ŠESTÁK, J.; KAHLE, V.

RIV year

2013

Released

12. 12. 2013

ISBN

1213-7103

Periodical

Chemické listy

Year of study

107

Number

State

Czech Republic

Pages from

438

Pages to

440

Pages count

BibTex

@article{BUT103645,
  author="Jozef {Šesták} and Vladislav {Kahle}",
  title="High pressure modification of the simple automated liquid chromatographic system for splitless nano column gradient separations",
  journal="Chemické listy",
  year="2013",
  volume="107",
  number="s3",
  pages="438--440",
  issn="1213-7103"
}