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

Method:

Quantification of residual solvents in an API using DMSO SupraSolv for headspace gas chromatography (cat. 101900)

Merck:/Freestyle/LE-Lab-Essentials/Solvents/LE-Solvens for headspace Chromatographic Conditions.jpg


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

Ordering Number
Product
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®
 
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