SupraSolv® Solvents for Headspace GC |
Analysis of Residual Solvents in Actives, Excipients and Drug Products
Headspace gas chromatography is a very precise and well accepted method for the analysis of residual solvents in drug substances and products according to ICH, USP and Ph. Eur. However, residual solvents analysis by headspace gas chromatography imposes high requirements on the solvents used for sample preparation. Accurate analysis requires the use of very pure solvents with extremely low concentrations of the defined residual solvents.
Merck SupraSolv® headspace solvents are especially designed to meet the sophisticated needs of residual solvents analysis by headspace gas chromatography: high purity and extremely low concentrations of the residual solvents as defined by the ICH.
SupraSolv® Headspace Solvents Offer
- High application reliability thanks to thorough application tests for every batch produced
- Application-oriented quality thanks to specified concentrations of residual solvents as defined by the ICH – for reliable and accurate analytical results.
Since residual solvents in drug products pose a risk to human health, pharmaceutical companies are required to test all products and confirm that concentrations are below harmful limits. Permissible maximum values for residual solvents in drug substances are defined by the ICH (International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use). The ICH guideline Q3C "Impurities: Guideline for Residual Solvents" categorizes all residual solvents into three classes according to their harmfulness to human health, and defines permissible maximum concentrations in drug substances and products. Both the European Pharmacopoeia (Chapter 2.4.24) and United States Pharmacopoeia (Chapter <467>) refer to this guideline and recommend headspace GC as the method of choice for analyzing residual solvents. SupraSolv® solvents for headspace gas chromatography are optimized for this application.
SupraSolv® Headspace Specification
Merck offers an unrivaled application-oriented quality that helps you to achieve accurate and reliable analytical results.
For our headspace solvents we exactly specify the concentrations of the various residual solvents of the three classes defined in the ICH guideline. Additionally, we perform a headspace application test for every batch produced. This gives you the application reliability you need for your daily work. SupraSolv® high-purity solvents for headspace GC specify the maximum allowed concentration of every residual solvent defined by the ICH:
Extract of Specification | |
|---|---|
| Every residual solvent of class 1 acc. ICH | ≤ 1μg/g |
| Every residual solvent of class 2 acc. ICH | ≤ 10μg/g |
| Every residual solvent of class 3 acc. ICH | ≤ 50μg/g |
Chromatographic Conditions
Column: |
Fused silica capillary column, DB1, length 30m, ID 0.32mm, film 5μm |
|---|---|
Pressure: |
0.6 bar / 8 psi (Helium) |
Injection: |
Splitless, 150°C |
Headspace conditions: |
Thermostating temperature: 80°C Transfer and needle temperature: 130°C Thermostating time: 30 min Pressurization: 1.0 min Injection time: 0.04 min Withdrawal time: 0.2 min High pressure: 2 bar / 28 psi |
| Detection: | FID, 250°C |
| Temperature: | 50°C for 5 min, with 8°C/min up to 240°C, hold 240°C for 5 min |
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Method: |
Quantification of residual solvents in an API using DMSO SupraSolv for headspace gas chromatography (cat. 101900) |
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Chromatographic Data
No. |
Compound |
Time (min) |
Area |
|---|---|---|---|
1 |
methanol | 2.0 | 12361 |
2 |
ethanol 3.8 | 3.8 | 399046 |
3 |
2-propanol | 5.4 | 2368 |
4 |
tert-butyl methylether | 9.0 | 34637 |
| 5 | diisopropyl ether | 10.5 | 43000 |
| 6 | tetrahydrofuran | 11.4 | 14083 |
| 7 | toluene | 11.5 | 11502 |
Ordering Information
Related Resources
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