A General LC-MS/MS Method for Monitoring Potential β-Lactam Contamination in Drugs and Drug-Manufacturing Surfaces

AAPS J. 2018 May 15;20(4):70. doi: 10.1208/s12248-018-0224-7.

Abstract

Penicillins and some non-penicillin β-lactams may cause potentially life-threatening allergic reactions. Thus, possible cross contamination of β-lactams in food or drugs can put people at risk. Therefore, when there is a reasonable possibility that a non-penicillin product could be contaminated by penicillin, the drug products are tested for penicillin contamination. Here, a sensitive and rapid method for simultaneous determination of multiple β-lactam antibiotics using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and validated. Mass spectral acquisition was performed on a Q-Exactive HF mass spectrometer in positive ion mode with parallel reaction monitoring (PRM). The method was validated for seven β-lactam antibiotics including one or two from each class and a synthetic intermediate. The quantification precision and accuracy at 200 ppb were in the range of ± 1.84 to ± 4.56 and - 5.20 to 3.44%, respectively. The limit of detection (LOD) was 0.2 ppb, and the limit of quantitation (LOQ) was 2 ppb with a linear dynamic range (LDR) of 2-2000 ppb for all eight β-lactams. From various drug products, the recoveries of eight β-lactams at 200 and 2 ppb ranged from 93.8 ± 3.2 to 112.1 ± 4.2% and 89.7 ± 4.6 to 110.6 ± 1.9%, respectively. The application of the method for detecting cross contamination of trace β-lactams (0.2 ppb) and for monitoring facility surface cleaning was also investigated. This sensitive and fast method was fit-for-purpose for detecting and quantifying trace amount of β-lactam contamination, monitoring cross contamination in manufacturing processes, and determining potency for regulatory purposes and for quality control.

Keywords: LC-MS/MS; cross contamination; parallel reaction monitoring; penicillin; β-lactams.

MeSH terms

  • Anti-Bacterial Agents / analysis*
  • Anti-Bacterial Agents / chemistry
  • Chromatography, High Pressure Liquid / methods
  • Drug Compounding / instrumentation
  • Drug Compounding / methods
  • Drug Compounding / standards
  • Drug Contamination / prevention & control*
  • Equipment Contamination / prevention & control
  • Feasibility Studies
  • Humans
  • Limit of Detection
  • Reproducibility of Results
  • Tandem Mass Spectrometry / methods*
  • beta-Lactams / analysis*
  • beta-Lactams / chemistry

Substances

  • Anti-Bacterial Agents
  • beta-Lactams