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高效液相色谱法测定牛奶中四环素类抗生素

时间:2017-12-01 19:03来源:毕业论文
摘要:[目的] 建立高效液相色谱法测定牛奶中四环素、土霉素、金霉素、强力霉素抗生素残留的方法。【方法】本实验采用高效液相色谱配紫外分光检测器测定实验结果,原理是土霉素
摘要:[目的] 建立高效液相色谱法测定牛奶中四环素、土霉素、金霉素、强力霉素抗生素残留的方法。【方法】本实验采用高效液相色谱配紫外分光检测器测定实验结果,原理是土霉素、四环素、金霉素、强力霉素在紫外吸收下最大吸收波长,大约波长为355nm处有最大的吸收峰,因此一系列不同的检测器和前处理、流动相变化下会对检测结果达到不同的效果,从而得到我们所需要的实验结果。建立高效液相色谱法测定牛奶中四环素、土霉素、金霉素、强力霉素抗生素残留的方法。样品经Mcllvaine缓冲溶液提取、OASIS HLB固相萃取柱净化后,经高效液相色谱分析,选定色谱柱ODS—C18,5 Ixm,250mmx4,流速为1 mL/min,柱温为30℃ ,流动相为乙腈+甲醇+0.01mol/L草酸溶液(20+10+70),二极管阵列检测器,检测波长为355 nm,进样量为10uL。
[结果与结论]得到检验结果:土霉素、四环素、金霉素、强力霉素标准溶液浓度在1.0ug~10.0ug/mL范围内,其线形回归方程为分别为土霉素y=16.216x+0.956、四环素y=22.572x+0.2646、金霉素y=7.1432x+0.4448、强力霉素y=13.128x+0.3715,相关系数分别为土霉素R=0.9992、四环素R=0.9999、金霉素R=0.9996、强力霉素R=0.9997,表明线性关系良好。其回收率范围土霉素97.2~89.8%、四环素91.3~101%、金霉素92.6~82.2%、强力霉素88.6~96.3%;分别为土霉素0.0411mg/kg、四环素0.0295mg/kg、金霉素0.0932mg/kg、强力霉素0.0507mg/kg。浓度为2.0ug/mL,5.0ug/mL,10.0ug/mL时,土霉素、四环素、金霉素、强力霉素的相对标准偏差分别为土霉素3.41%、0.76%、0.54%(n=6)、四环素1.92%、0.70%、0.53%(n=6)、金霉素5.59%、3.07%、1.34%(n=6)、强力霉素2.29%、1.80%、1.21%(n=6)。确定本方法具有时间短、灵敏度高、准确度高、精密度好等优点。15890
关键字:高效液相法;四环素;强力霉素 源自六-维+论\文"网*加7位QQ3249.114 www.lwfree.cn
 [objective] To establish an HPLC method for the determination of tetracycline, oxytetracycline, chlortetracycline, doxycycline antibiotic residues in milk.
 [Method] In this study,using high performance liquid chromatography with ultraviolet detection  for the determination of the experimental results, the principle is maximum absorption wavelength of  oxytetracycline, tetracycline, chlortetracycline, doxycycline in the UV absorption have maximum absorption peak at a wavelength of 355nm, so a series of different detectors and pretreatment mobile phase changes will achieve different effects.and we can obtaine experimental results . To establish a high performance liquid chromatographic method for the determination of oxytetracycline, tetracycline, chlortetracycline , doxycycline 4 kinds of antibiotics residue method in milk.sample from the Mcllvaine buffer solution extraction, OASIS HLB solid phase extraction column purification, by high performance liquid chromatography,and selected column ODS—C18,5 Ixm,250mmx4,speed is 1 mL/min,the column temperature was 30℃,the mobile phase consisted of acetonitrile + methanol+0.01mol/Loxalic acid solution (20+10+70),diode array detector, detection wavelength of 355 nm, amount of sample for 10uL.
[Results and Conclusions] Test results: oxytetracycline, tetracycline, chlortetracycline, doxycycline standard solution concentration within 1.0ug ~ 10.0ug/mL, its linear regression equation foroxytetracycline y = 16.216x +0.956, tetracycline y= 22.572x+0.2646, chlortetracycline y =7.1432x +0.4448, the doxycycline y = 13.128x +0.3715, the correlation coefficient for oxytetracycline the R = 0.9992, tetracycline R = 0.9999, chlortetracycline R = 0.9996, strongneomycin R = 0.9997, show a good linear relationship. the recoveries range: Oxytetracycline 97.2 to 89.8%, tetracycline 91.3 to 101%, chlortetracycline 92.6 to 82.2% doxycycline, 88.6 to 96.3%; oxytetracycline 0.0411mg/kg,
tetracycline 0.0295mg/kgthe chlortetracycline 0.0932mg/kg, doxycycline 0.0507mg/kg. when the concentration are  2.0ug/mL, 5.0ug/mL the, 10.0ug/mL, relative standard 高效液相色谱法测定牛奶中四环素类抗生素:http://www.lwfree.cn/shiping/20171201/17011.html
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