SupraSolv® solvents for headspace gas chromatography
For the analysis of residual solvents in actives, excipients and drug products according to ICH, Ph. Eur. and USP
Headspace gas chromatography is a very precise and well accepted method for the analysis of residual solvents in drug substances and products according to the ICH (International Conference of Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use), USP and Ph. Eur.
One challenge when working with headspace gas chromatography is to find a solvent quality that does not interfere with the analysis because it contains undefined levels of residual solvents. Merck Millipore SupraSolv® headspace solvents are especially designed for 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.
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Developed and specified in accordance with international standards
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 guideline Q3C “Impurities: Guideline for Residual Solvents”. This guideline divides 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. SupraSolv® solvents for headspace gas chromatography are optimized for this application.
Outstanding solvent quality
Merck Millipore offers an incomparable 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.
Table 1: 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 |
| Application: Quantification of residual solvents in an API | |
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| 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 temperaure: 80°C transfer and needle temperature: 130°C thermostating time: 30 min pressurisation: 1.0 min injection time: 0.04 min widthdrawal 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 |
| Method: | Quantifiation of residual solvents in an API using DMSO SupraSolv® for headspace gas chromatography (cat. 101900) |
| Chromatographic Data | |||
|---|---|---|---|
| No. | Compound | Time (min) | Area |
| 1 | methanol | 2.0 | 12361 |
| 2 | ethanol | 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 |
Result: the use of 1.01900 Dimethyl sulfoxide for headspace gas chromatography SupraSolv® for sample preparation leads to perfect separation performance and accurate results.
| Focus products | |
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| 1.00399 | N,N-Dimethylacetamide for headspace gas chromatography SupraSolv® |
| 1.00202 | N,N-Dimethylformamide for headspace gas chromatography SupraSolv® |
| 1.01900 | Dimethyl sulfoxide for headspace gas chromatography SupraSolv® |
| 1.00577 | Water headspace gas chromatography SupraSolv® |
Find out more about solvents for headspace gas chromatography SupraSolv®
