https://doi.org/10.15255/KUI.2005.028
Published: Kem. Ind. 56 (2) (2007) 53–56
Paper reference number: KUI-28/2005
Paper type: Conference paper
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HPLC-MS Analysis of Chloramphenicol Residues in Milk and Powdered Milk Products

A. Krivohlavek, L. Barušić, Z. Šmit, J. Bošnir and D. Puntarić

Abstract

Chloramphenicol (CAP) is a broad-spectrum antibiotic with bacteriostatic action but also has toxic properties, which is why its presence in food and feed is prohibited in Croatia and the European Union. In the aim of consumer protection it is essential to develop a sensitive analytical method for detection of CAP fractions lower than w = 0.3 μg kg–1. For the efficient control and monitoring of CAP, a rapid, sensitive, and selective method for its identification and quantification, using high performance liquid chromatography in combination with mass spectrometry LC-MS, has been developed. The cleaning procedure was based on the AOAC official method 993.32. HPLC-MS analysis used the ODS Hypersile column and the water/acetonitrile gradient. Electrospray negative ionization (neg ESI) was used before single ion monitoring (SIM) detection of three m/z 321, 323 and 325. As additional criteria, the ratio between these masses in real and spiked milk samples was also investigated in accordance with theoretical values of the isotope pattern for 2 chlorine atoms present in the analyte. The detection limit of 0.1 μg kg–1 was achieved. The mean value of recovery was 94 %, the correlation coefficient of the calibration curves calculated for 2 m/z values was higher than 0.99. Fourty samples of milk and milk products were tested with the HPLC-MS method, and obtained results showed that samples had CAP 0.37, 0.29, 0.39 μg kg–1, respectively. All the other analysed samples contained CAP concentrations below the detection limit.

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Keywords

chloramphenicol, liquid chromatography, mass spectrometry, milk