CEI-MS-12 — procedure

§4Procedure

The procedure below is written in the second person, which is the only place in the Institute's document set where that register is used. A procedure is an instruction and is written as one.

1. Establish which solvents are relevant from the synthesis and purification route. Where the route is not disclosed, run the full class 1 and class 2 screen and record that the route was not disclosed.
2. Prepare matrix-matched standards at the concentration limit for each solvent.
3. Weigh sample into headspace vials in duplicate and add diluent. Seal immediately.
4. Equilibrate at the stated temperature for the stated time. Both must be identical for samples and standards.
5. Inject headspace and acquire. Identify by retention time against standards and confirm by a second column or by mass-selective detection where a class 1 solvent is detected.
6. Quantify against the matrix-matched calibration.
7. Report each solvent detected, its concentration in parts per million, and its ICH limit. Report solvents screened and not detected as not detected, with the limit of detection stated.

References cited on this page

References are numbered in order of first citation in this document. Each superscript in the text links to its entry below.

1. International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use. ICH Q3C(R9) Impurities: Guideline for Residual Solvents. ICH Harmonised Guideline 2024;Step 4 version. identifier not held by the Institute

Identifiers are reproduced only where the Institute holds them. Where a digital object identifier or PubMed identifier is not shown, the Institute has recorded the journal and year and has not constructed an identifier.