Steroid Quantitative Charge Tags for LC-MS Analysis

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Solution Overview

Problem

Current methods for global steroid analysis in biological samples face challenges due to the diversity of steroids, lack of strong chromophores or ionized functional groups, and scarcity of quantitative standards, limiting the effectiveness of mass spectrometry techniques like GC-MS and LC-MS.

Innovation Solution

The use of quantitative charge tags based on Girard P and Girard T reagents, which allow for the labeling and detection of steroids with and without ketone groups, enabling simultaneous analysis in LC-MS through differential or isobaric mass tagging, facilitating the differentiation and quantification of various steroids.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If GC-MS is used for steroid analysis, then volatility and detection capability are improved, but steroid sulphates and cholesterol esters cannot be analyzed due to lack of volatility

Engineering Contradiction:
Improvedetection capabilityVSAvoidanalysis scope
Core Design Contradiction:
Measurement precisionVSAdaptability or versatility

Solution Approach 1:

The patent applies parameter changes by derivatizing steroids with Girard P or Girard T reagents, which chemically modify the steroid molecules to introduce charged groups. This transformation changes the physical and chemical parameters of the analytes, enabling them to be detected by mass spectrometry without requiring volatility, thus resolving the limitation of GC-MS for non-volatile steroid derivatives.

Inventive Principle:
Principle #35Parameter changes

2Adaptability or versatility

If LC-MS is used for steroid analysis, then analysis of non-volatile steroids is enabled, but sensitivity to neutral steroids is reduced and fragment-ion spectra are uninformative

Engineering Contradiction:
Improveanalysis scopeVSAvoidsensitivity
Core Design Contradiction:
Adaptability or versatilityVSMeasurement precision

Solution Approach 1:

The patent uses Girard P and Girard T reagents as intermediary substances that react with steroid ketone groups to form charged derivatives. These reagents act as mediators that bridge the gap between neutral steroids and the ionization requirements of mass spectrometry, enhancing sensitivity and providing informative fragment-ion spectra while maintaining the ability to analyze non-volatile steroids.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Measurement precision

If isotope dilution mass spectrometry with stable-isotope labelled standards is used, then quantification accuracy is improved, but the method becomes impractical for global steroid analysis

Engineering Contradiction:
Improvequantification accuracyVSAvoidmethod complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent applies universality by developing a single derivatization protocol using Girard P or Girard T reagents that can be applied to multiple different steroid analytes simultaneously. This universal approach eliminates the need for separate stable-isotope labelled standards for each individual steroid, reducing method complexity while maintaining quantification accuracy through the use of common internal standards.

Inventive Principle:
Principle #6Universality (Multi-functionality)

4Measurement precision

If multiple separate analyses are performed for different steroid types, then detection specificity is improved, but analysis time and instrument usage increase

Engineering Contradiction:
Improvedetection specificityVSAvoidanalysis throughput
Core Design Contradiction:
Measurement precisionVSProductivity

Solution Approach 1:

The patent merges the analysis of different steroid types into a single LC-MS run by using a universal derivatization protocol. All steroid analytes are derivatized with the same reagent system, allowing them to be analyzed simultaneously in one injection, thereby maintaining detection specificity while dramatically improving analysis throughput and reducing instrument usage.

Inventive Principle:
Principle #5Merging (Combining)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This approach enables the quantitative detection of multiple steroids in a single LC-MS run, improving throughput and reducing instrument time, while maintaining sensitivity and specificity, even in complex mixtures like plasma samples.

Implementation Method 1

The use of quantitative charge tags based on Girard P and Girard T reagents, which allow for the labeling and detection of steroids with and without ketone groups

Methodology Applied
Scientific EffectChemical Bonding: Chemical Bonding

Implementation Method 2

enabling simultaneous analysis in LC-MS through differential or isobaric mass tagging

Methodology Applied
Scientific EffectChromatography: Chromatography

Implementation Method 3

enabling simultaneous analysis in LC-MS through differential or isobaric mass tagging

Methodology Applied
Scientific EffectIonisation: Ionisation

Data Source

PatentEP2893355B1Kit and method for quantitative detection of steroids
Publication Date: 2019.06.05 UNIVERSITY COLLEGE OF SWANSEA
  • EP2893355B1 patent drawingFigure 1A~1C
  • EP2893355B1 patent drawingFigure 1D~1E
  • EP2893355B1 patent drawingFigure 2A

AI summary

The invention relates to a kit and methods for quantitative detection of steroids in a sample. The kit comprises quantitative charge tags and an oxidising agent.