Analysis of N-methylpyrrolidine in cefepime hydrochloride by ion chromatography using suppressed conductivity detection with solid-phase extraction pre-treatment

Abstract

N-Methylpyrrolidine (NMP) is the principal hydrolysis product of cefepime hydrochloride, a β-lactam antibiotic. Here we develop a sample preparation method for NMP in cefepime hydrochloride which significantly improves the stability of sample solutions.

Reactions of MoCl5 and MoO2Cl2 with Succinimide, 1, 4-Diaminobutane, 3-Methylpyridine, 1, 3-Diaminopropane, Pyrazole and 1- Methylpyrrolidine in Tetrahydrofuran

“…It is present in cigarette smoke. It is part of cefepime 42 : broad-spectrum cephalosporin antibiotic capable to treat bacteria causing pneumonia, infections of the skin and urinary tract. Desired properties 27,43 on transition metals for particular applications can be incorporated by coordination of metals with certain ligands.…”

Advanced analytical methods and sample preparation for ion chromatography techniques

“…For the practical performance of solid-phase extraction, many manufacturers offer ready-to-use cartridges lled with sorbent materials (Table 4) as well as devices for passing the sample solution through the sorbent bed either manually, semiautomatically or fully automatically. [59][60][61] There are great demands for the trace analysis in many scientic disciplines, requiring correspondingly sensitive methods to improve IC detection performance. With the currently available instrument congurations in IC technique, numerous ions can be routinely determined without any great difficulty even in concentration ranges below 1 mg L À1 .…”

Rapid determination of N-methylpyrrolidine in cefepime by combining direct infusion electrospray ionisation-time-of-flight mass spectrometry with field asymmetric waveform ion mobility spectrometry

“…The preparation of a cefepime sample for analysis therefore requires either the extraction of the NMP from the cefepime matrix to minimise the contribution from NMP produced by degradation in solution prior to analysis, or rapid analysis of the sample solution before signicant degradation occurs. 11 A further challenge in the determination of NMP in cefepime is that the singly and doubly protonated cefepime generated by electrospray mass spectrometry (ESI-MS) are readily fragmented in the intermediate pressure region of the mass spectrometer interface by collision-induced dissociation (CID), also known as in-source CID, to form protonated NMP. The NMP generated by CID interferes with response from the protonated NMP formed from NMP present in the cefepime sample, since NMP resulting from the sample and via CID cannot be distinguished by mass spectrometry alone.…”