Analytical method of residual oxytetracycline in apple juices using HPLC

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  • Shotaro Hirata
    Division of Hygienic Chemistry, Osaka Institute of Public Health Graduate School of Sustainable System Sciences, Osaka Metropolitan University
  • Masayama Atsushi
    Division of Hygienic Chemistry, Osaka Institute of Public Health
  • Nakatani Tadashi
    Division of Hygienic Chemistry, Osaka Institute of Public Health
  • Hoshi Hidenobu
    Graduate School of Sustainable System Sciences, Osaka Metropolitan University

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Other Title
  • HPLC を用いたりんごジュース中オキシテトラサイクリンの残留試験法
  • HPLC オ モチイ タリン ゴジュース チュウ オキシテトラサイクリン ノ ザンリュウ シケンホウ

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Description

An analytical method using HPLC was developed to analyze residual oxytetracycline (OTC) in apple juices. Residual OTC was extracted with a citrate-phosphate buffer containing EDTA-2Na. The matrix was removed from the extract by a solid-phase column, InertSep PLS-2 (265 mg/20 mL). After removing the solvent, the extract was resolved in a potassium phosphate solution. OTC in the test solution was determined quantitatively using HPLC with a photodiode array detector (PDA). The interfering peaks were not observed in chromatograms of blank extracts, indicating the high selectivity of this method. The limit of quantification of this method was 0.01 µg/g in apple juices. Method validation was performed by recovery tests at 0.2 µg/g to evaluate the trueness, repeatability (RSDr), and with-in laboratory reproducibility (RSDwr). The validation results for two types of apple juice exhibited sufficient recovery (99% and 85%) and precision (RSDr ≦ 4% and RSDwr ≦ 5%). The time required for the preparation of eight test solutions was less than three hours. This method can help inspect residual OTC in apple juices.

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