高效液相色谱法测定牛奶及牛可食性组织中咪唑苯脲
Determination of Imidocarb Residues in Bovine Edible Tissues by High-Performance Liquid Chromatography
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摘要: 建立了高效液相色谱法(HPLC)测定牛奶及牛可食性组织中咪唑苯脲(IMD)残留.牛奶或已匀浆组织先用β-葡萄糖苷酶水解，组织用盐酸超声提取，再用提取液萃取，牛奶直接用提取液提取.用乙腈-戊烷磺酸钠水溶液作为流动相，经高效液相色谱C18柱分离后用紫外检测器检测.咪唑苯脲质量浓度在0.01～10.00 μg/mL的范围内呈现良好的线性关系，相关系数大于0.999；组织加标样品检出限为0.01 μg/g,定量限为0.02 μg/g.在定量限、最高残留限量、2倍最高残留限量添加水平下的平均回收率为80.02%～114.72%，批内相对标准偏差为0.83%～10.92%，批间相对标准偏差为7.45%～12.69%.表明该检测方法简单、灵敏、可靠，适用于牛奶及牛组织中咪唑苯脲残留的分析.Abstract: A confirmative method has been developed to determine imidocarb(IMD) residues in edible tissues and milk of bovine by high-performance liquid chromatography(HPLC).The tissues and milk were first hydrolyzed by β-glucosidase. The tissues were extracted with hydrochloric acid, ultrasonicated and back-extracted with extract while the milk was extracted with extract only. The mobile phase was acetonitrile and 1-pentansulfonic acid sodium salt solution. The analyte was detected by UV absorptive spectroscopy after separation by C18 column. The range of linearity was 0.01-10.00 μg/mL; the relevant coefficient was more than 0.999. The limit of detection (LOD) was 0.01 μg/g, and the limit of qualification(LOQ) was 0.02 μg/ g. Mean recoveries from bovine tissues and milk fortified at LOQ, MRL(the maximum residue limit) and 2MRL were from 80.02%-114.72%, whereas the corresponding RSDs were from 0.83%-12.69%. In conclusion, the established method is simple, sensitive and reproducible for the determination of imidocarb residues in edible tissues and milk of bovine.
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Keywords:
- high-performance liquid chromatography /
- imidocarb /
- residue /
- milk /
- edible tissue of bovine
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