高效液相色谱法测定牛奶及牛可食性组织中咪唑苯脲

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0.01～10.00μg/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0.01μg/g,定量限为0.02μg/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.

Determination of Imidocarb Residues in Bovine Edible Tissues by High-Performance Liquid Chromatography

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.