Determination of Amidoxime Antibiotic Residues in Edible Silkworm Pupae
A liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was established for the determination of residues of four acylamide antibiotics,namely chloramphenicol,thiamphenicol,florfenicol and florfenicol amine in edible silkworm pupae.The samples were extracted with acetonitrile containing 1%ammonia water,dehydrated with anhydrous sodium acetate and anhydrous magnesium sulfate,purified with C18 adsorbent,and dissolved in pure water after nitrogen drying.The target compounds were separated by Eclipse Plus C18(2.1 mm×100 mm,1.8 μm)chromatographic column under the mobile phase of 0.05%ammonia aqueous solution and methanol,detected by multi-reaction monitoring(MRM)under positive and negative ion modes of electric spray ion source,and quantitative analyzed by isotope internal standard method.The experimental results show that chloramphenicol had a good linear correlation in the concentration range of 0.025-1.000 μg/L.The correlation coefficient(r)was 0.9990.The average recovery rate of chloramphenicol was 99.1%-108.6%,and the relative standard deviations(RSDs)were 3.3%-7.0%.Thiamphenicol,florfenicol and florfenicol amine had a good linear correlation in the concentration range of 0.125 μg/L to 5.000 μg/L.The correlation coefficients were≥0.9920.Their average recovery rates were 89.5%-112.1%,and RSDs were 3.6%-15.8%.This method offers rapid,accurate,and sensitive detection,making it suitable for the analysis of the aforementioned antibiotics in edible silkworm pupae.
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