Micro-SPE (μSPE) emerged as an automated green micromethod for sample preparation and clean-up in food safety, proteomics, forensic, environmental and analysis since more than ten years. Applications are wideranging and cover drugs, environmental contaminants, and, in particular, the extract clean-up in multiresidue pesticide analysis. The automation of the μSPE sample preparation steps led to the desired standardization of the applied sorbent materials for extract clean-up for the large variety of food commodities, an increase in sample throughput, and the welcome potential for offline and online hyphenation with GC-MS, LC-MS or even IC analysis.

This report presents for the first time the application of µSPE for the clean-up of the raw extracts using ethyl acetate as extraction solvent for pesticides from different also more complex food commodities.

Herein, we describe the development of a new high-throughput approach based on the newly introduced SampleStream Platform for performing clone selection screening, enabling selection of clones that produce the highest amount and quality of the correctly assembled bispecific antibody.
 

An efficient method for the generation and GC-analysis of FAME was generated using PAL Method Composer ver. 1.4. PAL Method Composer allows to rapidly generate methods by simple drag & drop operations.

Using a sandwich injection mode with the PAL LCMS-P tool enables improvements in peak shape and chromatography for samples containing a high percentage organic composition when injected into a high aqueous mobile phase.

A standardized automated workflow is suggested using a regular industry-standard x,y,z-robotic system for the individual derivatization steps at different reaction temperatures. The reagent addition, timing of the derivatization steps and analysis are controlled by the robotic system.

A completely automated Nitrosamine extraction method as per specified by FDA for Direct Injection and Headspace can be performed on the same PAL RTC.

 Due to the high dynamic range of different metabolites, SWATH/MS data acqusition allows the quatification on both precursor and product ion level including flexibility of the quantifier choice.
 

The distinctive onion and fruity odorous compounds were detected by both static headspace and ITEX-DHS techniques.

In the described experiments the precise injection of a pesticide solution in acetonitrile at 10 ng/mL, as it is the typical situation after a QuEChERS extraction and clean-up, was demonstrated with both the "Fast" liquid band injection and the "Normal" hot needle injection.

Pipetting suspensions for process control in chemical production

Gins are essentially neutral spirits flavoured with various botanicals by compounding or by distillation. The combination of HS-SPME Arrow with GCxGC-MSD/FID is a very powerful tool in the comparative analysis of samples with complex matrices.

The automatization not only eliminates manual lab work, it also allows an automated elaboration of optimized conditions for transesterification.

Here we present a facile and robust method how to boil and then analyze rice samples in a fully automated fashion.

A fully automated, true green analytical method, for high sensitivity and precision pesticide analysis. This report describes for the first time a fully automated QuEChERS extraction and clean-up workflow for homogeneous matrices like fruit juices, demonstrated for orange juice.

This article describes the routine screening method for 57 odorous compounds in drinking water. It uses the versatile SPME ARROW extraction on a PAL RTC System to screen and quantify odorous substances in drinking water.

A method for the quantitative analysis of 9 polycyclic and nitro musk fragrances from fish samples by PAL SPME Arrow and GC-MS/MS has been developed.

The method outlined above allows to fulfill requirements for the analysis of residual ethylene oxide and 2-chloroethanol as stated in GB 19083-2010.

The presented method allows a time-efficient sensitive detection and quantification of glyphosate, AMPA and glufosinate in
complex food matrices by applying online SPE.

The aim of this work was the determination of an optimal SPME fiber for extraction of boar taint causing compounds. For this purpose, different SPME fibers were tested and compared with respect to their extraction performance.

The steps outlined in this Appl Note should help you to quickly identify and eliminate carry-over when using the PAL LCMS-P Tool.

High-throughput, high sensitivity and low carryover: the new infusion automation from Trajan LEAP Automation offers you everything you need to bring your lipidomics mass spec workflow to its peak performance.

The described SPME Arrow GC-MS method for off-flavors is not only simple in operation and automated, but also fast and accurate, and satisfies completely the hygienic test requirements of drinking water and water source control in the China hygienic standard of drinking water (GB5749-2006).

This App Note illustrates how Smart Sampling with EBIS helps to run labs more efficiently.

Hair testing is a powerful tool routinely used for the detection of drugs of abuse in forensic and toxicology applications.

This application note highlights the versatility of the PAL System platform for performing different SPME experiments

Automated sample preparation reduces the costs per sample and avoids sample handling errors. This is especially important in therapeutic drug monitoring or diagnostics based on blood samples.

Highly efficient automation due to the PAL DHR Dual Head instrument under the CHRONOS control software. The system analyzes a sample in 45 minutes.  The Clean-Technology provides excellent robustness of the 
system.

Here we describe the quantitative analysis of iodoform in tap water by PAL SPME Arrow extraction combined with GC/MS. Immersion as well as headspace SPME has been performed on two different fiber types. The PAL SPME Arrow is a new technology for microextraction, combining trace level sensitivity with high mechanical robustness.

The obvious advantage of the SPME/GC-MS method to analyze stale aldehydes in beer gives a rapid extraction and better separation with small sample volumes. It is a very suitable solution for the monitoring of the status of beer aging and keep it as its best quality.

Automated enrichment and clean-up prior to liquid chromatography mass spectrometry (LC-MS) analysis using online SPE is demonstrated.

This study developed real time monitoring of off-flavours using a functionalized auto sampler with SPME-GC-MS.

This application note describes a simple and quick thermal desorption (TD) based approach for the sampling and analysis of target compounds (phthalates) in plastic toys and childcare articles.

The automation of the entire sample preparation process, incl. online injection on the PAL RTC achieves excellent results and high productivity. Using a mixed mode μSPE cartridge enables the efficient class separation of lipids (i.e. neutral and phospholipids).

This work presents a fully automated workflow using a workstation with robotic tool change (RTC) based on a method using sodium methoxide in methanol as reactant.

PAL SPME Arrow is a suitable tool for fulfillment of the German standard method DIN 38 407-41 for headspace-solid-phase microextraction of volatile analytes from aqueous samples.

This study demonstrated the application of an automated high-throughput mini-SPE cleanup for the  analysis of pesticides and environmental contaminants in QuEChERS extracts of foods.

This application note describes the automated gravimetric dilution of (viscous) samples.

This article presents a new approach to the use of mid infrared range (MIR) transmission spectroscopy in the context of bioprocess engineering.

ITEX DHS Application Notes for Environmental, Chemical and Food Safety analysis

A method for the quantitative analysis of a number of different N-nitrosamines from aqueous samples has been worked out.

HDX experiments are an example of where automation has great value. The requirement for significant investment of time in the data processing tasks places very high emphasis on obtaining the best quality experimental data. Variance and potential mistakes inherent in manual experimental technique result in wasted effort processing poor data.

Demonstration of a routine analytical method for the quantitation of volatile organic compounds in drinking water, using the
TriPlus RSH ITEX system along with a Thermo Scientific™ ISQ™ 7000 MS system coupled with a Thermo Scientific™ TRACE™
1310 Gas Chromatograph (GC) and Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS). Method linearity
and detection limits were assessed to evaluate method performance.

Automation of the digestion step provides a number of advantages, in particular for reproducibility, purity and time consumption. Unlike most other sample preparation systems the PAL RTC allows the preparation of smaller sample batches, which suites the medium-throughput requirements of a proteomic laboratory.

Process oil samples automatically – increase throughput

Building sample prep workflows - what does it take. In this article we will look at the analysis of fatty acids as an example.

This note covers the development and use of miniaturized cSPE for QuEChERS.

The method employing a SPME Arrow allows for the quantitation of water samples down to 50 ng/L for most of the described aldehydes with good precision.
A previous publication applying traditional standard SPME fibers and GC/MS achieved sensitivities down to 120-340 ng/L in spiked samples for C1, C3-C5

While syringes can dispense liquids with high accuracy and precision they are less practical when different solvents or higher amounts need to be dispensed. The PAL Dilutor Tool is designed to bridge this gap.

The automated Bligh and Dyer extraction described here was found to not only be more time efficient, but also to improve repeatability and quality of extraction and separation when compared to the standard manual approach.

In drug discovery, knowing the distribution of parent drug and metabolites in tissue sections is a crucial step. Presently, the particular molecular forms and quantities of the drug-related materials present must be determined from punched samples of areas of interest.

The article presents a dilution method developed to prepare calibration curves. The method is explained and results obtained with the method are shown.

In this App Note we focused on in-tube extraction (ITEX) as a powerful alternative to classic purge & trap analysis. The approach is particularly well suited for the analysis of trace organic compounds with a wide range of volatilities. Due do the simplicity of the system, it can be applied successfully to the analysis of heavily loaded samples without the risk of cross contamination and permanent system failure.

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Essential for sample preparation

Automated μSPE cleanup for GC-MS or LC-MS analysis of pesticides and environmental contaminants in QuEChERS extracts of foods

PAL Pipetting Tool - Essential for Life Science and Clinical Applications

Three new LC-MS Tools, all equipped with Smart Syringes.

Maintaining and preparing your syringe are two of the most important aspects to guarantee your PAL System can provide reliable results. This Article shows you the tips and tricks to adequately preapre your syringe for use as well as to prolong the lifetime.

General Information for PAL Smart Syringes

General Information for PAL Smart SPME Arrows

General Information for PAL Smart SPME Fibers

General Information for PAL SPME Fibers

CTC Analytics processes have incorporated the results from internal and external evaluation to ensure compliance with the EU RoHS regulation.

CTC Analytics supports the substitution of unnecessary hazardous chemicals and strives to eliminate all use of Substances of Very High Concern (SVHC) if possible or otherwise communicate the presence of SVHC in our supply chains.

CTC Analytics supports the goal of ending violence, human rights violations and environmental devastation in the Covered Countries. We are committed to complying with all requirements applicable to our Company under the Conflict Minerals Rule. CTC Analytics complies with US - Dodd-Frank Act known as the ''Conflict Minerals Rule".

Our products convince through quality and innovation. We implement demanding development projects. In doing so, we maintain active cooperation with technology partners, suppliers and universities. We align our company processes with the ISO standard EN 13485.

The PAL Compendium

This compendium on instrumental sample preparation showcases the many proven solutions of automated sample preparation workflows for food, environmental, pharma, life science analysis, and beyond. 

Automated μSPE cleanup for GC-MS or LC-MS analysis of pesticides and environmental contaminants in QuEChERS extracts of foods

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Sustainability is a key part of our strategy/values -this already since the foundation of the company in 1984. It is deeply anchored in our business activities and investment decision-making. Our commitment goes far beyond compliance with legal requirements. We are convinced that a careful use of resources is key to our long-term success. Consequently, we live a very sustainable culture in our company, which shapes the decisions and behavior of our employees.

• Appication of µSPE in Routine Pesticide
• Automated Sample Prep for FAME analysis
• New arrivals for the LC-MS tool familiy
• New arrival 20 µL Pipetting Tool
• New arrival Dilutor tool DX with 80 mm needle

• Bispecific Antibody Clone Selection
• New Tools for LC-MS
• New Tools for LC-MS Sample Prep
• Tray Cooler: One for all samples

• Metabolite Profiling by Automated Methoximation and Silylation
• Nitrosamines in Pharmaceuticals
• New Version of PAL Method Composer

• Drinking Water Quality Control - Screening for 57 Odorous Substances using SPME Arrow
• New arrivals - PAL Centrifuge

Since more than ten years micro-SPE (µSPE) emerged as a micromethod for sample preparation and clean-up in food safety, proteomics, forensic, environmental and analysis. Applications are wide-ranging and cover drugs, environmental contaminants, and, in particular, the QuEChERS extract cleanup in multiresidue pesticide analysis. The automation of the µSPE sample preparation steps led to the desired increase in sample throughput, unification of the used sorbent materials for food commodities, and the potential for the online hyphenation with GC-MS and LC-MS instrumentation.
 

Using PAL Robotic Tool Change (RTC) system, a fully automated QuEChERS was developed for the extraction and clean-up of organochlorine and organophosphate pesticides from homogeneous samples. The automated QuEChERS workflow includes extraction with acetonitrile, salting out with
saturated sodium chloride solution and the clean-up with PAL μSPE prior to injection into the GC-MS/MS for analysis.

The μSPE direct injection workflow has been optimized and used for the high-throughput cleanup of liquid samples. Several μ-SPE cartridges are currently being tested by LCMS for the cleanup of complex sample matrices containing various pesticides and drugs, in order to further validate the performance of the direct μ-SPE-LCMS workflow in different use cases.

The μ-SPE clean-up efficiency was demonstrated in the removal of matrixinterfering components and in the recovery of pesticides.

The automated mini-SPE clean-up workflow improved the efficiency of analysis and significantly increased the sample throughput.

In our study we evaluate the available filtration options for x-y-z robots and some not-yet commercially available filtration devices prototypes.

The goal of this development was to establish a generic clean-up procedure for the extracts of the ethylacetate extraction method which is useful for all incoming food types without requirement for different clean-up procedures dedicated to different food types.

The objective was to establish an automated µSPE clean-up procedure for PAH analysis in edible oils, here used sunflower oil. We were using the greater concepts of Green Analytical Chemistry and automation.

The automatization not only eliminates manual lab work, it also allows an automated elaboration of optimized conditions for transesterification.

This work presents a fully automated workflow using a workstation with robotic tool change (RTC based on a method using sodium methoxide in methanol as reactant .The workflow improves process safety, optimizes throughput and minimizes handling error.

The analysis of volatile organic compounds (VOCs) is a faster approach to identify the honey’s origin than traditional methods, which is important for the quality control of honeys. In-tube extraction dynamic headspace (ITEX-DHS) is a fully automated microextraction technique, in which the enrichment of analytes takes place by repeated aspiring and dispensing of the sample headspace through a sorbent trap

We have adapted a manual in-gel digestion protocol, including reduction, alkylation and acid-labile detergent assisted trypsin digestion of proteins, to be performed on a PAL RTC autosampler system.

A standardized automated workflow is suggested using a regular industry-standard x,y,z-robotic system for the individual derivatization steps at different reaction temperatures. The reagent addition, timing of the derivatization steps and analysis are controlled by the robotic system.

A severe drawback of offline SPE is the time consuming sample preparation. Online SPE circumvents this and enables complete automating of the SPE-LC-MS/MS workflow.

Static headspace for the main volatiles and HS-SPME extraction are combined in one workflow for comprehensive analysis of main and trace components.

Fully automated SPME Arrow immersion technique with GC/MS analysis is an excellent option to analyze PAH compounds in drinking water; with higher throughput and robustness

A fully automated, true green analytical method, for high sensitivity and precision pesticide analysis. This report describes for the first time a fully automated QuEChERS extraction and clean-up workflow for homogeneous matrices like fruit juices, demonstrated for orange juice.

The PAL system provides an affordable and reliable platform optimised for medium-throughput peptide preparation for shotgun-proteomics based mass spectrometry.

The automated ITEX Dynamic Headspace unit demonstrated equivalent accuracy and precision when compared to purge and trap and overall was more sensitive than the other enrichment techniques. The ITEX unit allows for automated analysis and optimization of conditions which drastically reduces analyst’s time when compared to performing the experiments manually with the purge and trap without any reduction in sensitivity, accuracy and reproducibility.

The use of lipidomic analyses based on LC-mass spectrometry has become widespread due to its sensitivity and specificity which provides a broader picture of lipid profiles in biofluids. In this work, we combined an automated sample extraction and a two-dimensional liquid chromatography (2DxLC) system with HILIC-based class separation followed by an orthogonal reverse-phase chromatography with an untargeted SWATH-DIA workflow to accurately annotate phosphatidylcholines (PC), lysophosphatidylcholine (LPC) and etherphosphatidylcholines (PC O-) in human plasma samples.

In this poster presentation, we compare two workflows for the cleanup of multi-class veterinary drugs in animal tissue matrices, based on the Thermo Scientific™ VetDrugs Explorer Collection (P/N VDX-TSQ02-10001, Thermo Fisher Scientific, Waltham MA, USA).

Applying the automated workflow described, the analyst’s time to prepare samples and standards, and then optimize conditions was drastically reduced when compared to performing the experiments manually without any reduction in accuracy and reproducibility. At the same time the automated procedure enabled complete traceability of every step.

In the present work were evaluated the use of UHPLC-MALDI-MS/MS for the analysis of metabolites of talinol generated in-vitro.

Here we propose to integrate an automated Bligh and Dyer extraction on a robotic system including a dual-column UHPLC-MS/MS platform for the metabolomic analysis of tissues or cells. The aqueous fraction is split and analysed sequentially at two different mobile phase pH values, whereas the lipidic fraction is analysed alternately with an extended gradient.

Carry-over is the appearance of an analyte signal in a blank after the analysis of samples with higher analyte concentrations. It is compound and method dependent. Minimal carry-over is an important quality criterion of modern auto sampler technology and critical in HT-Analysis. In this study a strategy to minimize carry-over for HT-analysis was developed.

A workflow is described that enables the automated selection of the most suitable extraction conditions (type of fiber, extraction time and temperature) for the GC/MS analysis of a number of contaminants in oil and water samples.

for PAL LC-Systems

The performance of SPME fibers is an essential aspect of an analytical method. This study shows the comparison of three different SPME fibers of a conventional brand  and the new PAL SPME Fibers.

Would you like to automate your sample preparation workflow or injection (LC or GC)?

Solid Phase Micro-Extraction (SPME) is widely used for chemical analysis of foods, beverages and food contact materials. As an automated technique, the SPME applications are selected for their simplicity, throughput and extraction efficiency.  As a solvent-free extraction, it is gains even more importance today as a green analytic technique. Besides the traditional SPME Fiber, the new SPME Arrow is enhancing trace level sensitivity at high mechanical robustness. With these features, this presentation will give insight on SPME analysis in coffee, wine and off-flavors. 

Presented by:

Erich Leitner, Graz University of Technology Institute of Analytical Chemistry and Food Chemistry

Stefan Cretnik, PhD, Product Manager, CTC Analytics AG

Extraction of volatile compounds is a widely used approach for analysis of foods and beverages.  By the nature of gas phase sampling, the limiting factor for polar analytes are given by low vapor pressure or higher boiling points of semi-volatile compounds. These limitations can be overcome by sampling at decreased pressure levels using vacuum conditions. This has been shown in several publications using vacuum sampling techniques. In this study, a fully automated approach of Vacuum In-Tube Extraction (V-ITEX) is presented, a simple and fully automated technique using PAL system autosamplers. The application examples include flavors, fragrances, off-flavors, pesticides and biomarkers by extractions directly from the food sample matrix, such as Honey, Bee Wax, Cheese, Onions, Blood and Urine.  

Presented by:

Pascal Fuchsmann, Head of Flavor Analytics Agroscope

Stefan Cretnik, Product Manager CTC Analytics AG

Recent developments in pesticides analysis extend the well-established methods to higher productivity and reliability while minimizing consumption and exposition to harmful chemicals. A workflow was developed that allows automatic preparation of calibration standards, automatic sample dilution, and automatic clean-up of sample extracts on one instrument, showing that miniaturized automated solutions are reducing errors, improving analytical consistency and protecting the environment in one convenient approach.

Presented by:

Thomi Preiswerk, Senior Account Manager, CTC Analytics AG

Gwen Lim , Specialist for automated sample preparation, CTC Analytics

Ederina Ninga, Postdoc, Research Group for Analytical Food Chemistry, Danish Technical University 

This webinar offers a close insight into the operation and latest developments of automated SPME for VOCs and SVOCs by headspace, direct immersion and derivatization techniques. Key applications for food, water, environmental and forensic samples for use in every laboratory for GC-MS and LC-MS, also direct MS analysis are discussed.

Presented by:
Hans-Joachim Huebschmann, PhD

This presentation focuses on Sample Preparation aspecting in Metabolomics and Lipidomics

Presented by:
David Ruskic and Prof. Gerard Hopfgartner, Life Sciences Mass Spectrometry, Department of Inorganic and Analytical Chemistry, University of Geneva

In this presentation we want to discuss an important development and a demand from analytical laboratories about the standardization and the automation of sample preparation procedures for food safety, environmental, the forensic or pharmaceutical analysis.

Presented by:
Hans-Joachim Huebschmann, PhD

The QuEChERS analysis method is a popular solid-phase extraction method used for the analysis of pesticide residues in food. However, there are analytical and logistical limitations during cleanup. The Webinar shows two workflow variations for high sample throughput in online GC-MS and LC-MS analysis. 

Presented by:
Hans-Joachim Huebschmann, PhD, Gwen Lim and Chiew Mei Chong, CTC Analytics AG

For metabolite profiling chemical derivatization has been used to improve MS sensitivity and LC retention. However, for multi-analytes quantification, the number of available isotopically labelled internal standards is limited. And, there is no single workflow which can provide large-scale metabolomics coverage in particular for polar metabolites.

Presented by:
Prof. Gerard Hopfgartner, Life Sciences Mass Spectrometry, Department of Inorganic and Analytical Chemistry, University of Geneva

• Learn about the importance of fundamental aspects of sample preparation and modern, sustainable sample preparation technologies
• Find out about the latest innovations in sample preparation in environmental analysis
• Learn about new materials used in sample preparation

Presented by:
Günter Boehm, PhD, VP Sample Prep Solutions, CTC Analytics AG

This webinar features practical aspects in the daily routine of SPME Arrow, and aspects for the comparison towards SPME Fibers. Application examples will include VOCs, PAHs, Fragrances and Off-flavours.

Presented by:
Stefan Cretnik, PhD, Product Manager, CTC Analytics AG

See this detailed video of the µSPE workflow for the clean-up of raw pesticides extract. The µSPE cartridge is operated in scavenger mode eluting the pesticides in a clean extract. The matrix is kept on the sorbent material. The cleaned extract can be injected without waiting time online for LC-MS or GC-MS analysis. All samples are treated on the same time axis for highest reliability.