高效液相色谱法测定水产品中7种兽药残留量
HPLC Determination of Residual Amounts of 7 Veterinary Drugs in Aquatic Products
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摘要: 提出了高效液相色谱法同时测定水产品中呋喃唑酮、噁喹酸、萘啶酸及4种磺胺类药物等7种兽药残留量的方法。样品经乙腈提取,正己烷脱脂,用中性氧化铝柱和C18固相萃取柱进行分离及净化。以Symmetry C18色谱柱为分离柱,以不同体积比混合的乙腈与0.08 mol·L-1乙酸溶液为流动相进行梯度洗脱,紫外检测器于波长265 nm处检测。7种兽药的质量浓度与其峰面积均在0.05~1.0 mg·L-1范围内呈线性关系,检出限(3S/N)为0.01~0.04 mg·kg-1。方法的回收率在68.2%~97.3%之间,相对标准偏差(n=6)在1.6%~14%之间。Abstract: A method of HPLC for the determination of residual amounts of 7 veterinary drugs, including furazolidone, oxolinic acid, nalidixic acid and 4 sulfonamides in aquatic products was proposed. The sample was extracted with acetonitrile and defatted with n-hexane. The residue obtained was taken up with CH3CN-H2O (95+5) and purified by passing through neutral alumina column and C18 column. The eluate was separated on Symmetry C18 column by gradient elution with mixtures of acetonitrile and 0.08 mol·L-1 acetic acid solution in different ratios, and determined with UV detector at the wavelength of 265 nm. Linear relationships between values of peak area ad mass concentration of the 7 veterinary drugs were obtained in the same range of 0.05-10.0 mg·L-1, with detection limits (3S/N) in the range of 0.01-0.04 mg·kg-1. Values of recovery and RSD′s (n=6) of the method found were in the ranges of 68.2%-97.3% and 1.6%-14% respectively.