Simultaneous determination of 11 related impurities in propofol by gas chromatography/tandem mass spectrometry coupled with pulsed splitless injection technique

Abstract

A variety of related impurities, including starting materials, process impurities, and degradation products, can be detected in propofol. In this article, a sensitive and selective GC-MS/MS method using pulsed splitless injection technique for the determination of 11 main related impurities in propofol in one chromatogram is investigated. This method is extensively validated for its linearity, recovery, precision, LOD, and LOQ, and is able to detect trace-level related impurities (LOD = 0.2-5.6 μg/g) in propofol bulk drug. Stressed tests proposed that oxidative degradation, photolytic degradation, and heat are the main causes for the formation of degradation products in propofol.

A fast, fully validated GC‐MS method using a simplified pretreatment for the quantification of short and branched chain fatty acids in human stool

“…Setting the initial oven temperature 20°C lower than the boiling point of water allowed analyte focusing and formation of narrow bands on the column resulting in increased signal of all analytes 16,30,31 . Chromatogram A in Figure 4 shows the increase in mass detector responses for all analytes in XIC mode for a human stool sample as abundance compared to a typical 10:1 split injection in Chromatogram B. Acetic acid displayed the highest increase at 3:1 in abundance while the other analytes showed an increase of at least 2:1.…”

“…This finding may explain Setting the initial oven temperature 20 C lower than the boiling point of water allowed analyte focusing and formation of narrow bands on the column resulting in increased signal of all analytes. 16,30,31 Chromatogram A in Figure 4 3.4 | Linearity (r 2 ), sensitivity (as LLOQ), ULOQ, and LOD…”

Continuous Flow Synthesis of Propofol

“…The impurities profile for pharmaceutical compounds is fundamental for safety reasons, especially for intravenous drugs such as Propofol. Industrials processes allowing the Propofol have revealed the presence of numerous side products—which were detected by gas chromatography [ 25 ]—resulting from the synthesis and degradation, multiplying health’s risks and purification steps. Hence, to ascertain the purity level of the Propofol produced from our flow process, analyses by gas chromatography were performed.…”

Propofol solubilization and structural transformations in dilutable microemulsion

“…During the last decade a number of attempts to improve the quality of an emulsion loaded with propofol were made [5][6][7]. The emulsions that were used, in spite of FDA approval, had several major drawbacks: pain upon injection, physical instability, hyperlipidemia, oxidation, and the tendency for microorganism contamination [8][9][10]. Two major propofol emulsion producers were forced to discontinue their production because of severe problems with the emulsions that were marketed.…”