Chemical vapour deposition in narrow capillaries: Electro-osmotic flow control in capillary electrophoresis.

BACKGROUND: In capillary electrophoresis (CE), the inner surface of fused-silica capillaries is commonly covalently modified with liquid silanes to control electroosmotic flow (EOF). This liquid phase deposition (LPD) approach is challenging for long and narrow-diameter capillaries (≥1 m, ≤25 µm ID) inhibiting commercial production. Here, we use chemical vapour deposition (CVD) to covalently modify capillaries with different silanes. Using a home-built CVD device, capillaries were modified with neutral (3-glycidyloxypropyl) trimethoxysilane (GPTMS), the weak base (3-aminopropyl) trimethoxysilane (APTMS), the weak acid 3-mercaptopropyltrimethoxysilane (MPTMS) and the neutral hydrophobic trichloro(1H,1H,2H,2H-perfluorooctyl) silane (PFOCTS). Gas-phase modification of GPTMS with acid and ammonia allowed further modification of the surface prior to molecular layer deposition (MLD) of poly(p-phenylene terephthalamide) (PPTA) using the self-limiting sequential reaction between terephthalaldehyde (TA) and p-phenylenediamine (PD) vapours. RESULTS: Capillaries coated with GPTMS by CVD showed a greater reduction in EOF at all pH values than the conventional LPD. APTMS showed a reduction of the EOF at pH 9, with EOF reversal observed below pH 6. MPTMS provided a slightly lower EOF than an unmodified capillary at high pH, and a slightly higher EOF at lower pH. PFOCTS provided the most consistent EOF as a function of pH. The deposition of successive layers of PPTA resulted in increased surface coverage of the polymer and a greater reduction in EOF at pH higher than 5. The stability of a 10 µm ID GPTMS coated capillary was tested at pH 8.8 in a 200 mM CHES/Tris BGE for the separation of inorganic anions. Over 1.5 months of continuous operation (≈4130 runs), the reproducibility of the apparent mobilities for chloride, nitrite, nitrate and sulfate were 2.43%, 2.56%, 2.63% and 3.05%, respectively. The intra-day and inter-day column-to-column reproducibility and batch-to-batch reproducibility for all the coated capillaries ranged between 0.34% and 3.95%. SIGNIFICANCE: The study demonstrates the superior performance of CVD coating for suppressing the EOF compared to LPD allowing the easy modification of long lengths of narrow capillary. The variation in silane, and the ability of MLD to modify and control the surface chemistry, provides a simple and facile method for surface modification. The stability of these coatings will allow long-term capillary electrophoresis monitoring of water chemistry, such as for monitoring fertiliser run-off in natural waters.

Recent advances in miniaturization of portable liquid chromatography with emphasis on detection.

Liquid chromatography is a prominent analytical technique in separation science and chemical analysis, applied across numerous fields of research and within industrial applications. Over the past few decades, there has been a growing interest in the miniaturization of this technique, which has been particularly enabled through new miniature and portable detection technologies for in-field, at-site, and point-of-need (collectively 'out-of-lab') analyses. Accordingly, significant advances have been made in recent years in the development of miniaturized liquid chromatography with photometric, electrochemical, and mass spectrometric detection, enabling the development of field-deployable and portable instruments for various applications. Herein, recent developments in the miniaturization of detection systems for inclusion within, and/or coupling with, portable liquid chromatographic systems, are reviewed in detail together with critical comments and expected future trends in this area.

Evaluation of Analyte Transfer between Microfluidic Droplets by Mass Spectrometry.

Droplet microfluidics enables high-throughput experimentation and screening by encapsulating chemical and biochemical samples in aqueous droplets segmented by an immiscible fluid. In such experiments, it is critical that each droplet remains chemically distinct. A common approach is to use fluorinated oils with surfactants to stabilize droplets. However, some small molecules have been observed to transport between droplets under these conditions. Attempts to study and mitigate this effect have relied on evaluating crosstalk using fluorescent molecules, which inherently limits the analyte scope and conclusions drawn about the mechanism of the effect. In this work, transport of low molecular weight compounds between droplets was investigated using electrospray ionization mass spectrometry (ESI-MS) for measurement. The use of ESI-MS significantly expands the scope of analytes that can be tested. We tested 36 structurally diverse analytes that were found to exhibit crosstalk ranging from negligible to complete transfer using HFE 7500 as the carrier fluid and 008-fluorosurfactant as a surfactant. Using this data set, we developed a predictive tool showing that high log P and log D values correlate with high crosstalk, and high polar surface area and log S correlate with low crosstalk. We then investigated several carrier fluids, surfactants, and flow conditions. It was discovered that transport is strongly dependent on all of these factors and that experimental design and surfactant tailoring can reduce carryover. We present evidence for mixed crosstalk mechanisms including both micellar and oil partitioning transfer. By understanding the driving mechanisms, surfactant and oil compositions can be designed to better reduce chemical transport for screening workflows.

Compact capillary high performance liquid chromatography system for pharmaceutical on-line reaction monitoring.

Due to their size, conventional high performance liquid chromatographs (HPLCs) are difficult to place close to a reaction vessel within a pharmaceutical manufacturing or development site. Typically, long transfer lines are required to move sample from the reactor to the HPLC for analysis and high solvent usage is required. However, herein a compact and modular separation system has been developed to enable co-location of an HPLC with a small-scale reactor for reaction monitoring in the synthesis of active pharmaceutical ingredients. Using a framework based on capillary HPLC, a compact gradient separation system with a fully modular architecture is described. A custom miniature diode-array detector with a linear dynamic range (up to 1500 mAU at 210 nm) was integrated and evaluated for on-line reaction monitoring. In evaluating system suitability, average peak area %RSD of <3%, and an average retention time %RSD of <0.7%, were achieved. To demonstrate practical utility, the compact system was coupled directly to an on-line lab-scale flow through reactor for continuous reaction monitoring in the laboratory fume hood, where a study of the 3rd Bourne reaction was used to compare the performance of the compact system with a commercially available process HPLC instrument (Waters PATROL UPLC). Further, 33 off-line samples from a continuous crystallization reactor were analysed and it was found that the developed compact HPLC system showed equivalent quantitative performance to an Agilent 1290 Infinity II HPLC system.

Portable capillary electrophoresis coupled with swab-based extraction device for cleaning validation in pharmaceutical facilities.

All pharmaceutical manufacturers are required to verify that their production equipment is free from contaminants. Here, we report the capability of a fully automated portable capillary electrophoresis instrument with an integrated sample swab extraction - the Grey Scan ETD-100 - for the detection of pharmaceutical residues on surfaces of manufacturing equipment. Lidocaine was used as a model compound and could be recovered from a surface by swabbing, extracted from the swab, and analysed within 1 min. The recovery of lidocaine from a stainless-steel coupon was 81.3 %, with a LOD of 0.13 µg/swab. This fast, sensitive, and simple method implemented on a user-friendly portable CE instrument without the need for manual sample pre-treatment provides the possibility for on-site rapid determination of equipment cleanliness in the pharmaceutical industry.

Applications of covalent organic frameworks and their composites in the extraction of pesticides from different samples.

Pesticides are used extensively in a wide range of applications and due to their high rate of consumption, they are ubiquitous in the different media and samples like environment, water sources, air, soil, biological materials, wastes (liquids, solids or sludges), vegetables and fruits, where they can persist for long periods. Pesticides often have hazardous side effects and can cause a range of harmful diseases like Parkinson, Alzheimer, asthma, depression and anxiety, cancer, etc, even at low concentrations. To this end, extraction, pre-concentration and determination of pesticides from various samples presents significant challenges caused by sample complexity and the low concentrations of them in many samples. Often, direct extraction and determination of pesticides are impossible due to their low concentrations and the complexity of samples. The main goals of sample preparation are removing interfering species, pre-concentrating target analyte/s and converting the analytes into more stable forms (when needed). The most popular approach is solid-phase extraction due to its simplicity, efficiency, ease of operation and low cost. This method is based on using a wide variety of materials, among which covalent organic frameworks (COFs) can be identified as an emerging class of highly versatile materials exhibiting advantageous properties, such as a porous and crystalline structure, pre-designable structure, high physical and chemical stability, ease of modification, high surface area and high adsorption capacity. The present review will cover recent developments in synthesis and applications of COFs and their composites for extraction of pesticides, different synthesis approaches of COFs, possible mechanisms for interaction of COFs-based adsorbents with pesticides and finally, future prospects and challenges in the fabrication and utilization of COFs and their composites for extraction of pesticides.

Small footprint liquid chromatography-mass spectrometry for pharmaceutical reaction monitoring and automated process analysis.

Liquid chromatography (LC) has broad applicability in the pharmaceutical industry, from the early stages of drug discovery to reaction monitoring and process control. However, small footprint, truly portable LC systems have not yet been demonstrated and fully evaluated practically for on-line, in-line or at-line pharmaceutical analysis. Herein, a portable, briefcase-sized capillary LC fitted with a miniature multi-deep UV-LED detector has been developed and interfaced with a portable mass spectrometer for on-site pharmaceutical analysis. With this configuration, the combined small footprint portable LC-UV/MS system was utilized for the determination of small molecule pharmaceuticals and reaction monitoring. The LC-UV/MS system was interfaced directly with a process sample cart and applied to automated pharmaceutical analysis, as well as also being benchmarked against a commercial process UPLC system (Waters PATROL system). The portable system gave low detection limits (∼3 ppb), a wide dynamic range (up to 200 ppm) and was used to confirm the identity of reaction impurities and for studying the kinetics of synthesis. The developed platform showed robust performance for automated process analysis, with less than 5.0% relative standard deviation (RSD) on sample-to-sample reproducibility, and less than 2% carryover between samples. The system has been shown to significantly increase throughput by providing near real-time analysis and to improve understanding of synthetic processes.

Small-Footprint, Field-Deployable LC/MS System for On-Site Analysis of Per- and Polyfluoroalkyl Substances in Soil.

Per- and polyfluoroalkyl substances (PFASs) are emerging environmental pollutants of global concern. For rapid field site evaluation, there are very few sensitive, field-deployable analytical techniques. In this work, a portable lightweight capillary liquid chromatography (capLC) system was coupled with a small footprint portable mass spectrometer and configured for field-based applications. Further, an at-site ultrasound-assisted extraction (pUAE) methodology was developed and applied with a portable capLC/mass spectrometry (MS) system for on-site analysis of PFASs in real soil samples. The influential variables on the integration of capLC with MS and on the resolution and signal intensity of the capLC/MS setup were investigated. The important parameters affecting the efficiency of the pUAE method were also studied and optimized using the response surface methodology based on a central composite design. The mean recovery for 11 PFASs ranged between 70 and 110%, with relative standard deviations ranging from 3 to 12%. In-field method sensitivity for 12 PFASs ranged from 0.6 to 0.1 ng/g, with wide dynamic ranges (1-600 ng/g) and excellent linearities (R2 > 0.991). The in-field portable system was benchmarked against a commercial lab-based LC-tandem MS (MS/MS) system for the analysis of PFASs in real soil samples, with the results showing good agreement. When deployed to a field site, 12 PFASs were detected and identified in real soil samples at concentrations ranging from 8.1 ng/g (for perfluorooctanesulfonic acid) to 2935.0 ng/g (perfluorohexanesulfonic acid).

Biomass-derived carbon nanospheres decorated by manganese oxide nanosheets, intercalated into polypyrrole, as an inside-needle capillary adsorption trap sorbent for the analysis of linear alkylbenzenes.

Carbon nanospheres (CNSs) were derived hydrothermally from biomass (orange peels) and decorated by manganese dioxide (MnO2) nanosheets. The MnO2/CNSs nanocomposite was intercalated into polypyrrole (PPy) during flow-through in-situ electropolymerization of pyrrole on the surface of the inner wall of a stainless-steel needle to prepare an inside-needle capillary adsorption trap (INCAT) device. The surface morphology, thermogravimetric behavior, sorption characteristics, and structure of the MnO2/CNSs@PPy nanocomposite were characterized using scanning electron microscopy (SEM), thermogravimetric analysis (TGA), energy dispersive X-ray analysis (EDX), nitrogen physisorption by the Brunauer-Emmett-Teller (BET) method, dynamic light scattering (DLS) size distribution, and Fourier-transform infrared spectrometry (FT-IR). The INCAT device was coupled with GC-FID and applied for dynamic headspace analysis of linear alkyl benzenes (LABs) in wastewater samples. The effective experimental variables on the extraction efficiency was optimized using a central composite design (CCD) based on response surface methodology (RSM). Under the optimal conditions, the limits of detection (LODs) were in the range of 0.5-1.0 ng mL-1. The calibration plots were linear over the range of 0.01-10 µg mL-1. The relative standard deviations (RSDs%) for intra-day, inter-day, and inter-INCAT precision were calculated 5.3-8.3%, 9.4-13.5%, and 13.6-16.9%, respectively. The developed technique was employed successfully for the analysis of LABs in water and wastewater samples with average recovery values ranging from 92 to 109%. A single INCAT device was used more than 90 times without significant change in its extraction capability.

Corrigendum to "Ultra-trace determination of oxyhalides in ozonated aquacultural marine waters by direct injection ion chromatography coupled with triple-quadrupole mass spectrometry" [Heliyon 7 (4) (April 2021) e06885].

[This corrects the article DOI: 10.1016/j.heliyon.2021.e06885.].

Ultra-trace determination of oxyhalides in ozonated aquacultural marine waters by direct injection ion chromatography coupled with triple-quadrupole mass spectrometry.

A direct, robust, accurate and highly sensitive method for oxyhalide species in natural waters, including seawater, using suppressed ion chromatography coupled with mass spectrometry (IC-MS) is described. The method utilised a high capacity, high efficiency anion-exchange column (Dionex IonPac AS11-HC, 4 mm, 2 × 250 mm), with the separation achieved using an electrolytically generated potassium hydroxide gradient, delivered at 0.380 mL min-1. Applying the method, detection limits for iodate, bromate, and chlorate in seawater after direct sample injection (20 µL injection volume, samples diluted 10-fold), were 11, 30 and 13 ng L-1 (ppt), respectively. Standard addition calibrations to ozonated seawater samples were linear, in all cases R2 > 0.999 (n = 10), with intra-day repeatability of 3.7, 11.2 and 1.8 % RSD (n = 10) for a low-level standard mixture (0.30 µg L-1 of iodate, 0.15 µg L-1 of bromate, and 1.50 µg L-1 of chlorate). The method was applied to the analysis of seawater samples taken pre- and post-disinfection points within a recirculating aquacultural system. Iodate, bromate and chlorate were detected as the main oxyanionic disinfection by-products, demonstrating the practical utility of the new method as a valuable tool for monitoring changes to seawater composition following disinfection treatments.

Ultraviolet absorbance detector based on a high output power 235 nm surface mounted device-type light-emitting diode.

A new miniaturised capillary flow-through deep-UV absorbance detector has been developed using a microscale surface mounted device- type light-emitting diode (LED) (Crystal IS OPTAN 3535-series), emitting at 235 nm and with a half-height band width of 12 nm, and a high-sensitivity Z-shaped flow-cell. Compared with a previously reported TO-39 ball lens LEDs emitting at 235 nm, the new generation LED produced a 20-fold higher optical output and delivered up to 35 times increase in external quantum efficiency (EQE). The Z-cell was based on a reflective rectangular optical path with cross-sectional dimensions of 100 × 100 µm and a physical optical pathlength of 1.2 mm. Inclusion of UV transparent fused-silica ball lenses, between the SMD and the Z-cell, improved light transmission by a factor of 9 and improved the detector signal-to-noise ratio by a factor of 2.2, at the same input current. The detector was housed within an Al-housing fitted with a cooling fan and demonstrated excellent linearity with stray light down to 0.06%, and an effective pathlength of 1.1 mm (92% of nominal pathlength). The resultant detector was fitted successfully into a briefcase-sized portable capillary HPLC system, and practically demonstrated with the detection of a mixture of 13 test compounds at the sub-mg L-1 level in <5 min using gradient elution.

Miniature Multiwavelength Deep UV-LED-Based Absorption Detection System for Capillary LC.

A new miniature deep UV absorbance detector has been developed using low-cost and high-performance LEDs, which can be operated in both scanning (230 to 300 nm) and individual wavelength (240, 255, and 275 nm) detection modes. The detector is mostly composed of off-the-shelf components, such as LEDs, trifurcated fiber optic assembly, a capillary Z-type flow cell, and photodiodes. It has been characterized for use with a standard capillary LC system and was benchmarked against a standard variable wavelength capillary LC detector. The detector shows very low levels of stray light (<0.4%), utilization of up to 99.0% of the effective path length of the flow cell, a wide dynamic range (0.5 to 200 µg/mL for sulfamethazine, carbamazepine, and flavone), and low noise levels (at 300 µAU level). The detector was applied within a miniaturized LC system.

Modular, cost-effective, and portable capillary gradient liquid chromatography system for on-site analysis.

This work demonstrates the development of a compact, modular, cost-effective separation system configured to address a specific separation problem. The principles of the separation are based on gradient capillary liquid chromatography where the system consists of precision stepper motor-driven portable syringe pumps with interchangeable glass syringes (100 µL to 1000 µL). Excellent flow-rate precision of < 1% RSD was achieved with typical flow-rates ranging from 1 µL/min to 100 µL/min, which was ideal for capillary columns. A variable external loop volume and electrically actuated miniature injection valve was used for sample introduction. Detection was based upon a commercial Z-type UV absorbance flow-cell housed within a custom-built cooling enclosure (40 mm x 40 mm) which also contained a UV-LED light-source and a photodiode. System and chromatographic performance was evaluated using linear gradient elution, with day to day repeatability of <1.5% RSD (n = 6) for peak area, and < 0.4% RSD (n = 6) for retention time, for the separation of a 5 component mixture using a 50 mm X 530 µm ID C18 3 µm particle capillary column. The system can run any commercial or in-house packed columns from 50 mm to 100 mm length with IDs ranging from 200 to 700 µm. The developed portable system was operated using custom-built windows-based chromatography software, complete with data acquisition and system control.

Miniature and fully portable gradient capillary liquid chromatograph.

A robust, portable and miniature battery powered gradient capillary liquid chromatograph (total weight ∼2.7 kg, without battery ∼2.0 kg), with integrated microfluidic injection, column heating and high sensitivity low-UV absorbance detection is presented. The portable capillary chromatograph, was applied with a packed reversed-phase capillary column (100 mm × 300 µm I.D., 5 µm ODS), housed within an integrated capillary column heater controlled by a proportional-integral-derivative (PID) chip module. The system delivered retention time and peak area relative standard deviation in isocratic mode of <0.7% (n = 10) and <3.3% (n = 10), respectively, and <0.1% (n = 10) and <2.3% (n = 10) respectively, for gradient elution mode. Detection was based upon a 255 nm light-emitting diode (LED) using one of two commercial capillary flow-cell options, namely a high sensitivity 12 nL Agilent capillary z-cell (HSDC) and a 45 nL Thermo Fisher Scientific UZ-View™ flow cell (UZFC). The HSDC, housed within a 3D printed detector arrangement, gave an effective pathlength of 1.01 mm (84% of nominal pathlength) and stray light of only 0.2%. Limits of detection for four test small molecule pharmaceuticals ranged from 65 to 101 µg L-1 based upon a 316 nL injection volume, with separation efficiencies of between 18,000 and 29,700 N m-1, with sub-4 min run times. The portable capillary LC system was successfully coupled to a small footprint portable mass spectrometer (Microsaic 4500 MiD) to demonstrate compatibility and 'point-of-need' miniaturised LC-MS capability.

Localised quantitative structure-retention relationship modelling for rapid method development in reversed-phase high performance liquid chromatography.

Quantitative structure-retention relationships (QSRR) predicting the values of solute "hydrophobicity" coefficient η' in the approximate hydrophobic subtraction model (HSM) can be used to predict retention times of compounds on numerous reversed-phase (RP) columns, provided that column parameters on the corresponding stationary phases are available. In the present study, we propose a new dual clustering-based localised QSRR approach, combining P-ratio clustering (where P is the octanol-water partition coefficient) with second dominant interaction (SDI)-based clustering, to produce predictive models with an acceptable level of prediction accuracy for in silico column scoping in RP method development. QSRR models for η' values were derived for 49 compounds out of 63 in a dataset extracted from the literature, where retention data were measured under one isocratic mobile phase condition (i.e., acetonitrile-water, 50:50 [v/v]). These models gave a predictive squared correlation coefficient Qext(F2)2 of 0.83 and a root mean square error of prediction (RMSEP) of 0.14. For the modelling, a genetic algorithm-partial least square regression (GA-PLS) approach was performed using the η' values and their relevant molecular descriptors. The corresponding retention times were predicted by applying the predicted η' values of the models and the stationary phase "hydrophobicity" parameter H values for the corresponding columns to the approximate HSM, resulting in excellent accuracy and predictability (Qext(F2)2 of 0.90 and RMSEP of 0.72 min). The established QSRR approach was experimentally verified for six Thermo Scientific columns (Acclaim™ 120 C18, Acclaim Polar Advantage, Acclaim Polar Advantage II, Accucore™ aQ, Accucore Phenyl-X, and Hypersil Gold C18 columns) using two types of datasets. The first dataset consisted of eight model compounds extracted from the original dataset and retention time predictions for those compounds were then evaluated on the above columns. The result showed good agreement between predicted and observed retention times with an acceptable error in retention time predictions (slope of 0.97, Qext(F2)2 of 0.95, a mean absolute error (MAE) of 0.43 min and RMSEP of 0.61 min). The second dataset included eight test compounds not included in the original dataset, which were all classified into the η' cluster by applying a Tanimoto similarity (TS) threshold of 0.7. Similarly, predicted retention times of the test compounds were compared with their corresponding observed retention times, resulting in acceptable retention time predictions with the slope of 0.99, Qext(F2)2 of 0.93 and RMSEP of 0.52 min. Comparisons of resolution values between columns were utilised to select the most suitable columns for separations of the compounds in the respective test sets. Actual chromatograms obtained on the chosen columns showed the feasibility for effective column scoping without experimentation on numerous RP stationary phases available in the USP website, based on the predicted resolution values.

3D Printed Liquid Cooling Interface for a Deep-UV-LED-Based Flow-Through Absorbance Detector.

Ultraviolet (UV)-light-emitting diodes (LEDs) are now widely used in analytical absorbance-based detectors; as compared to conventional UV lamps, they offer lower cost, faster response time, and higher photon conversion efficiency. However, current generation deep-UV-LEDs produce excess heat when operated at normal operating currents, which affects output stability and reduces their overall performance and lifespan. Herein a 3D printed liquid cooling interface has been developed for a deep-UV-LED-based optical detector, for capillary format flow-through detection. The interface consists of a circular channel that is tightly wrapped around the LED to provide active liquid cooling. The design also facilitates easy plug-and-play assembly of the various essential components of the detector: specifically, a 255 nm UV-LED, a capillary Z-cell, and a broadband UV photodiode (PD). The unique liquid cooling interface improved the performance of the detector by reducing the LED temperature up to 22 °C, increasing the spectral output up to 34%, decreasing the required stabilization time by up to 6-fold, and reducing the baseline noise and limits of detection (LODs) by a factor of 2. The detector was successfully used within a capillary HPLC system and could offer a miniaturized, rapidly stabilized, highly sensitive, and low-cost alternative to conventional UV detectors.

Recent advances in open tubular capillary liquid chromatography.

This review covers advances and applications of open tubular capillary liquid chromatography (OT-LC) over the period 2007-2018. Under the right conditions OT-LC columns have the potential to offer superior column efficiency, higher overall peak capacity, and higher column permeability compared to packed capillary and monolithic columns. However, such advantages are highly dependent upon column format and dimensions, and to date in liquid chromatography the advantages of open tubular format columns have been most widely discussed and applied in the field of proteomics. In this review we have focused on the wider variety of separation mechanisms and applications which can be achieved following the modification of the inner wall of the capillary with a thin-layer stationary phase. In particular the latest advances in stationary phase development and formation, together with new column formats and dimensions are reviewed. Detection options for OT-LC are also discussed and recent advances in this area highlighted. Finally, this review summarises existing applications of OT-LC and illustrates the future potential for this technique.

Sub-1 mL sample requirement for simultaneous determination of 17 organic and inorganic anions and cations in Antarctic ice core samples by dual capillary ion chromatography.

The significant advance of delivering high value multi-species data from sub-1 mL ice core sample volumes allows higher temporal resolution in deposition records of inorganic and low molecular weight organic anions and cations. The determination of these species is a fundamental strategic requirement in modern paleoclimate studies. Herein, for the first time, a dual capillary ion chromatography (Cap-IC) based method for the simultaneous separation of 17 organic and inorganic anions and cations in low volume Antarctic ice core samples is presented. The total amount of sample required for direct injection has been reduced to 190 µL, which is 35 times lower than the amount of sample required by standard ion chromatography methods. A dual Cap-IC system configured for the simultaneous determination of cations and anions was used throughout. A range of chromatographic parameters was optimised for both anion and cation systems to obtain baseline separations of all target analytes in a suitable run time and to minimise the amount of sample required. Baseline separation of matrix and trace 'marker' ions were achieved in less than 35 min, after injecting only 40 µL of sample in each IC system. Limits of detection (LODs) for all analytes determined were within a range similar to that achieved by previously published standard bore IC-based methods. Intra- and inter-day repeatability were evaluated, with both parameters being typically below 3% for peak area. In further validation of the method, a comparative analysis of a set of 420 ice core samples from Aurora Basin North site, Antarctica, previously analysed by standard IC, established that the proposed low sample volume technique was applicable as a routine measurement approach in ice core analysis projects.