Simultaneous determination of nine aminoglycosides and tetracyclines antibiotics residues in crayfish by high performance liquid chromatography-tandem mass spectrometry
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摘要: 建立了龙虾中6种氨基糖苷类和3种四环素类抗生素残留的高效液相色谱串联质谱（HPLC-MS/MS）同时检测方法。样品中抗生素采用5%三氯乙酸-磷酸盐溶液提取,经超声萃取、固相萃取柱净化,C18色谱柱分离,对样品前处理条件、液相色谱分离条件和质谱检测条件进行了优化。通过实际样品添加回收率实验,链霉素、双氢链霉素、四环素、金霉素和土霉素定量检出限均为5μg/kg,庆大霉素、卡那霉素、新霉素和妥布霉素定量检出限均为50μg/kg,9种抗生素三个添加水平下,龙虾样品加标回收率在66.1%107.9%,相对标准偏差在0.7%9.7%。结果表明,该方法准确、高效,适用于龙虾中6种氨基糖苷类和3种四环素类药物残留的同时检测和确证。
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关键词:
- 高效液相色谱串联质谱 /
- 氨基糖苷类抗生素 /
- 四环素类抗生素 /
- 龙虾
Abstract: A method based on high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) had been developed for simultaneous determination of 6 aminoglycoside and 3 tetracycline antibiotics residues in crayfish. The antibiotics were ultrasonic extracted from crayfish muscles with 5% trichloroacetic acid-phosphate buffer solution,purified by hydrophilic-lipophilic balance(HLB) cartridge and separated by C_(18) chromatographic column. The pre-treatment method,chromatographic and MS/MS parameters were optimized.The limits of detection for streptomycin,dihydrostreptomycin,tetracycline,chlortetracycline and oxytetracy-cline were 5 μg/kg,respectively,and for gentamycin,kanamycin,neomycin andtobramycin 50 μg/kg,respectively.The recoveries of 9 antibiotics residues at three spike levels ranged from 66.1% to 107.9% with the relative standards deviations of 0.7%~9.7%. The established method was accurate and effective for confirmation and quantification of 9 different aminoglycoside and tetracycline antibiotics residues in crayfish.-
Keywords:
- HPLC-MS/MS /
- aminoglycosides /
- tetracyclines /
- crayfish
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