Application of On-Line Sorbentless Cryogenic Needle Trap Extraction Coupled with GC-FID for Analysis of Some Organic Volatile Impurities in Solid Pharmaceuticals.

Abstract

An automated sorbentless cryogenic needle trap device (ASCNTD) was developed for the extraction of organic volatile impurities (OVIs) from solid pharmaceuticals prior to their determination by gas chromatography (GC). In this method, a new set up was designed and used to extraction of several OVIs from ceftazidime, ceftriaxone sodium and amoxicillin. For this purpose, a proper amount of the sample was transferred into the extraction vessel. The sample headspace components were started to circulate through a needle with a flow rate of 20mLmin-1. The OVIs were trapped on the inner surface of a needle placed on top of the sample by flowing liquid nitrogen. After a predetermined time, the coiled nichrome resistance wire placed into the hollow ceramic rod was heated and the trapped analytes were desorbed and swept into the GC capillary column using the carrier gas. The effective parameters such as volume of the sample vial, headspace flow rate, extraction temperature and time, and desorption conditions have been investigated. Qualification studies reveal that pyridine (as a degradation product of ceftazidime), methylene chloride, diethylamine, triethylamine, isopropyl alcohol and n-butyl acetate are the main impurities in the studied pharmaceuticals. Detected OVIs were quantitated using external standard method. The obtained relative standard deviation values were <8%, and the limits of detection (LOD) for the detected OVIs were in the range of 1-34ngg-1.