흰다리새우(Litopenaeus vannamei)에서 cephalexin의 잔류농도 연구를 위한 LC-MS/MS 분석법 연구
Analytical method study for cephalexin with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) applicable for residue studies in the whiteleg shrimp Litopenaeus vannamei
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초록
Cephalexin, a semi-synthetic cephalosporin antibiotic, has long been used in fish aquaculture in various countries under legal authorization. The drug is thus widely available for use in other aquatic species except fishes like the crustacean whiteleg shrimp. This study aims to develop a sensitive method for laboratory residue studies to adopt in withdrawal period determinations. Through repeated trials from the existing methods developed for other food animal tissues, it was possible to achieve a sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method. The results showed that at a concentration of 0.1 mg/kg, the recovery rate was 81.79%, and C.V. value was 8.2%, which meet the recovery rate and C.V. recommended by Codex guideline. After satisfactory validation of analytical procedures, applicability to the shrimp tissue was confirmed in experimentally cephalexin-treated whiteleg shrimp. As a result, most muscle samples were detected below the limit of quantification (0.05 mg/kg) after day 3, and most hepatopancreas samples were detected below the limit of quantification after day 14. In particular, the limit of quantification 0.05 ppm with the presently developed method suggests sufficient sensitive over the current legal maximum residue limit of 0.2 mg/kg set for fishes.
Abstract
Cephalexin, a semi-synthetic cephalosporin antibiotic, has long been used in fish aquaculture in various countries under legal authorization. The drug is thus widely available for use in other aquatic species except fishes like the crustacean whiteleg shrimp. This study aims to develop a sensitive method for laboratory residue studies to adopt in withdrawal period determinations. Through repeated trials from the existing methods developed for other food animal tissues, it was possible to achieve a sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method. The results showed that at a concentration of 0.1 mg/kg, the recovery rate was 81.79%, and C.V. value was 8.2%, which meet the recovery rate and C.V. recommended by Codex guideline. After satisfactory validation of analytical procedures, applicability to the shrimp tissue was confirmed in experimentally cephalexin-treated whiteleg shrimp. As a result, most muscle samples were detected below the limit of quantification (0.05 mg/kg) after day 3, and most hepatopancreas samples were detected below the limit of quantification after day 14. In particular, the limit of quantification 0.05 ppm with the presently developed method suggests sufficient sensitive over the current legal maximum residue limit of 0.2 mg/kg set for fishes.
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