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Application Note ReView: AS246: Simulant Solution Extraction Using Automated Dispersive Liquid-Liquid Microextraction (DiLLME) in Extractables & Leachables Analysis

Anatune

8th February 2022

DiLLME, DiLLME Analyser,


Simulant solutions are widely used in extractables & leachables analysis within the pharmaceutical and Electronic Nicotine Delivery System (ENDS) industries, as well as in testing of food contact materials for non-intentionally added substances (NIAS).

The simulant solution mimics the extractive properties of the in-use formulation, and is used to determine the nature and estimated amount of any substances which migrate from the packaging material to the drug product, e-liquid formulation, or foodstuff.

There are several challenging aspects to the sample extraction and analysis of simulant solutions, including:

  • Require solvent exchange and enrichment using harmful solvents in large quantities
  • Some simulant solutions are highly complex, often containing salts or detergents
  • Coupled with the need for, in many cases, very low limits of detection and quantitation
  • Traditional, non-automated sample extraction methods can lead to quantitative errors and risk contamination of the extract solution.

 

DiLLME, analyser, gerstel, mps, extractables & leachables, analysis

Anatune DiLLME Analyser & GERSTEL MPS Autosampler

 

Therefore this edition of Application Note ReView takes a look at AS246 from last year; an important App Note detailing Anatune’s highly-efficient Dispersive Liquid-Liquid Microextraction method for the automated extraction and enrichment of simulant solutions prior to chromatographic analysis.

This method delivers an automated solution provides significant advantages. These include:

  • Maintaining consistent precision over manual or semi-manual liquid extraction techniques used for sample prep in Extractables and Leachable analysis
  • Improving sample integrity and limits of detection
  • Obtaining more accurate and repeatable screening data
  •  Reducing analysis times.

 

How does it do this?

Dispersive Liquid-Liquid MicroExtraction (DiLLME), is a solvent extraction method that utilises a secondary dispersive solvent to both increase extraction efficiency and reduce sample mixing times. This enables it to achieve significant enrichment factors and reduce contamination.

Application Note AS246 demonstrates the capabilities and potential of DiLLME when applied to a variety of matrices and chemical classes for screening of Simulation Solutions in Extractables and Leachables analysis. It shows how the sensitivity specification was improved, and the excellent recovery of analytes with a wide range of concentrations demonstrates that, when combining extracts at both high and low pH, the method is entirely suitable for non-targeted analysis.

 

gertsel, mps, standalone, robotic, autosampler, annatunne, analysis,

 

GERSTEL MPS Autosampler 

 

As the entire sample extraction is automated via the Gerstel MPS system, reproducibility is assured. The risk of sample contamination is significantly reduced. With reasonably complex sample preparation operations such as this, the automation of the extraction process also saves operator time and, significantly, the low extraction solvent volumes (1 mL) reduce the environmental impact, cost and safety risks associated with the method.

And despite the requirement for LVI, intra-sample replicate analysis and, if necessary, repeat analysis is possible due to the volume of the final extract and sample storage in a temperature-controlled environment.

Whilst this application is concerned with extraction of Simulation Solutions, the automated sample extraction of test articles and subsequent back extraction using a variety of solvents and/or pH manipulation is also possible.

 

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