Development, validation and application to real samples of a liquid chromatography with tandem mass spectrometry method for the determination of tetracyclines in beeswax

Abstract

Beeswax is a valuable honeybee product, which finds applications in the food and pharmaceutical industries, as well as in cosmetic production. However, some substances used in apiculture, like tetracyclines, can be delivered to hives where they cause contamination of honeybee products such as beeswax. Tetracyclines are commonly used for the treatment of American and European foulbrood diseases, but in the European Union their usage by beekeepers is forbidden. Thus, a sensitive method for the analysis of tetracyclines in beeswax is an important analytical tool. A new liquid chromatography with tandem mass spectrometry method for the analysis of tetracyclines including oxytetracycline, 4-epioxytetracycline, tetracycline, 4-epitetracycline, chlorotetracycline, 4-epichlorotetracycline, and doxycycline in beeswax was developed. The method involved dilution of beeswax in n-hexane after a melting step, liquid-liquid extraction with oxalic acid and clean-up using a weak cation exchange phase. Satisfactory separation was performed on an octadecyl column with 0.1% formic acid and acetonitrile in a total run time of 5 min. The application of this method was evaluated by the analysis of real beeswax samples. The presence of oxytetracycline was confirmed in 5 out of 48 tested beeswax samples, which shows the method can be successfully used to determine the tetracyclines in beeswax.

Determination of tetracycline residue in pork by differential pulse voltammetry using activated glassy carbon electrode

“…[4][5][6] Most analytical methods commonly have been used for identifying and quantifying TC residues in animal-origin foodstuffs based on liquid chromatography coupled with a tandem mass spectrometry (LC-MS/MS). [7,8] However, the methods involve complex methods which require high-cost equipment, trained technician, and complex sample processing. Developing quick and reliable procedures for TC quantitative analysis is critical for government agencies.…”

Preparation of restricted‐access material precolumns by grafting δ‐gluconolactone onto a hybrid silica monolithic column for on‐line solid‐phase extraction of tetracycline residues from milk

“…To ensure food safety and human health, FAO/WHO, EU and China have provided the maximum residue limits for TCs as 0.1 mg/kg . In order to accurately determine TCs residues in foods, the separation analysis methods of HPLC and HPLC‐MS/MS have been developed . However, most samples usually have much more complex compositions.…”