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作 者:安琼 徐龙 王丽娜 李倩 王贞香 AN Qiong;XU Long;WANG Lina;LI Qian;WANG Zhenxiang(Hexi University Medicine College,Zhangye 734000;Key Laboratory of Hexi Corridor Resources Utilization of Gansu,Zhangye 734000)
机构地区:[1]河西学院医学院,张校734000 [2]甘肃省河西走廊特色资源利用重点实验室,张掖734000
出 处:《食品工业》2024年第7期310-316,共7页The Food Industry
基 金:甘肃省高等学校创新基金项目(2021A-120);甘肃省教育科技创新项目(2022B-172,2022B-205);甘肃省大学生省级创新训练项目(S202110740011,S202010740001)。
摘 要:运用AHP-CRITIC混合加权法确定正交试验中的各个影响因素的权重系数,并结合正交试验结果优选富集鸡肉样品中常用抗生素的最佳浊点萃取体系;建立测定鸡肉中抗生素的高效液相色谱法(HPLC)。考察不同表面活性的类型、表面活性剂的浓度、NaCl、HCl对富集吉他霉素、金霉素、土霉素的浊点萃取体系的影响,基于单因素用正交试验优化,对获得的结果,用层次分析(AHP)法、CRITIC法、AHP-CRITIC综合评价,获得富集吉他霉素、金霉素、土霉素最佳浊点萃取体系;建立测定吉他霉素、金霉素、土霉素的高效液相色谱法,对方法进行验证,用于真实样品的测定。结果表明,浊点萃取体系为TritonX-114浓度20%、温度50℃、酸浓度0.3 mol/L、NaCl浓度0.5 mol/L。优化色谱条件为Intersil C_(18)(4.6 mm×250 mm, 5μm)色谱柱,柱温30℃。吉他霉素的检测波长231nm,金霉素和土霉素的检测波长355 nm,流动相乙腈-0.2%的磷酸(85∶15,体积比)水溶液。金霉素、土霉素、吉他霉素的线性R~2均大于0.999,加样回收率均大于80.0%, S_(RSD)<5.0%。构建的浊点萃取体系能较好从鸡肉中富集金霉素、土霉素、吉他霉素,建立的HPLC方法能快速准确测定样品中抗生素含量。AHP-CRITIC mixed weighting method was used to determine the weight coefficient of each influencing factor in the orthogonal experiment,and combined with the results of the orthogonal experiment to optimize the optimal cloud point extraction conditions for the enrichment of common antibiotics in chicken samples,and a better antibiotic pretreatment technology was obtained.Establish a high performance liquid chromatography(HPLC)method for determination of antibiotics in chicken.Using TRITONX-114-114,NaCl and HCl,a turbid point extraction system with enrichment of kitamycin,aureomycin and oxytetracycline was constructed.The optimal turbid point extraction system with enrichment of kitamycin,aureomycin and oxytetracycline was obtained by orthogonal optimization and comprehensive evaluation of AHP,CRITIC and AHP-critic.The HPLC method for the determination of guitamycin,aureomycin and oxytetracycline was established.The method was verified and used for the determination of real samples.The results showed that turbidity point extraction system was 20%TritonX-114,temperature 50℃,acid concentration of 0.3 mol/L,and NaCl concentration of 0.5 mol/L.The optimized chromatographic conditions were as follows:Intersil Cig column(4.6 mmx250 mm,5μm)at 30℃.The detection wavelength of guitamycin was 231 nm,and that of aureomycin and oxytetracycline was 355 nm.The linear R’of aureomycin,oxytetracycline and kitamycin were all greater than 0.999.The recovery rate was over 80.0%,and Srsp was less than 5.0%in acetonitrile-0.2%phosphoric acid(85:15,volume ratio)aqueous solution.The established turbidity point extraction system can enrich aureomycin,oxytetracycline and guitamycin from chicken well,and the established HPLC method can quickly and accurately determine the content of antibiotics in samples.
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