HPLC DETERMINATION OF RESIDUAL SULFANILAMIDES IN FISH
摘 要
建立了鱼肉中5种磺胺类药物的高效液相色谱测定方法.样品经二氯甲烷提取,正己烷脱脂后经固相萃取柱净化等预处理.用Cloversil C18色谱柱,流动相为乙酸+甲醇+水(1+10+89)进行梯度洗脱,在紫外检测波长265 nm处,检出限可达0.1 μg·kg-1,线性范围为0-500 μg·L-1,相关系数大于0.999 3,样品加标回收率在78.6%-87.6%之间,测定结果的RSD在3.42%-9.03%之间.
Abstract
HPLC was applied to the determination of 5 residual sulfanilamides in fish,after its extraction with dichloromethane,de-fatting with n-hexane,and purification by solid-phase extraction on Waters Oasis HLB solid-phase extraction column.Sulfanilamides on the column were eluated with methanol,which was dried at 35 ℃ under reduced pressure.The residue was taken up with 1.0 mL of a mixture of CH3OH,CH3COOH and H2O (33+0.67+66.33),and the solution was used for HPLC analysis.HPLC separation was carried out on a Cloversil C18 column (250 mm×4.6 mm,i.d 5 μm),using a mixed solution of HOAC+CH3OH+H2O (1+10+89 by volume) as the mobile phase (phase A);and gradient elution with CH3OH at different volume ratios.UV detections were made at 265 nm.Linearity of the calibration curves of all the 5 sulfanilamides were in the range from 0 to 500 μg·L-1 with correlation coefficients largers than 0.999 3.Detection limits obtained were 0.1 μg·kg-1.Recoveries found were in the range of 78.6%-87.6%,and RSD′s ranged from 3.42% to 9.03%.
中图分类号 O657.37
所属栏目 试验与研究
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收稿日期 2005/8/9
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备注李孟玻(1977-),女,广东阳江人,硕士研究生,检验员,从事食品检验研究工作.
引用该论文: LI Meng-bo,ZHANG De-yun,PENG Zhi-jian,ZHAO Mou-ming. HPLC DETERMINATION OF RESIDUAL SULFANILAMIDES IN FISH[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2006, 42(8): 611~613
李孟玻,张德云,彭之见,赵谋明. 高效液相色谱法测定鱼肉中残留磺胺类药物[J]. 理化检验-化学分册, 2006, 42(8): 611~613
被引情况:
【1】郑春巍,刘洋,王启辉,周晓萍, "超高效液相色谱法测定畜禽肉中10种磺胺类药物残留量",理化检验-化学分册 48, 79-81(2012)
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参考文献
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【2】徐淮海.水产品中14种磺胺类药物残留的HPLC法同时测定[J].分析测试学报,2004,23(5):122-124.
【3】李俊锁.鸡肝组织中磺胺类药物多残留分析法[J].畜牧兽医学报,2002,33(5):468-472.
【4】蒋定国.畜禽肌肉、内脏及虾中磺胺二甲嘧啶残留量的检测技术研究[J].中国食品卫生杂志,2003,15(6):492-495.
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