Static headspace-GC analysis of ten residual solvents in water by using Shimadzu GC-2010 combined with Teledyne Tekmar HT3 static/dynamic headspace autosampler. Part 1. Precision of Analysis.

Introduction

Residual solvents present in bulk or finished pharmaceuticals are commonly analyzed according to the procedures specified in an international standard, such as the United States Pharmacopeia (USP). The USP 29 Chapter <467> describes the analysis method by using static headspace-gas chromatography with flame ionization detector. Although the chapter also describes other analytical procedures that may be used where specified in the individual monographs, the headspace operating parameters described in the main procedures indicate the use of automatic headspace sampler with a sample transfer line. Shimadzu GC-2010 gas chromatograph can be combined with the Teledyne Tekmar HT3 Static/Dynamic Headspace Sampler, which is an automated headspace sampler that uses a transfer line for transferring the headspace to the gas chromatograph. We used the static option of the headspace auto-sampler in the present work. Precision of the response (i.e. peak area) is one of the main parameters used in validating a system or in any quantitative routine work. We analyzed ten organic solvents at two concentration ranges to demonstrate the precision of the above system, namely of 2 to 5 ug/mL and 100 to 300 ug/mL. From the experiments that we have carried out both in our Singapore and India laboratories, we found that the %RSD values are within the USP specification of no more than 15%.

December 15, 2006 GMT