摘要
本研究建立了能同时测定牛奶中阿苯达唑、氟苯达唑、噻苯达唑及4种代谢物残留量的高效液相色谱定量分析方法。样品用10mL乙腈提取,取5mL提取液氮气吹干后,用10%盐酸溶液溶解,用C18固相萃取柱净化,净化液注入高效液相色谱仪,经C18反相色谱柱分离后,在紫外波长292nm处进行测定,外标法定量。结果表明,7种化合物在0.05~100μg/mL范围内线性关系良好,相关系数均≥0.9998;噻苯达唑检出限为0.025mg/kg,定量限为0.10mg/kg,5-羟基噻苯达唑等6种化合物检出限为0.05mg/kg,定量限为0.20mg/kg;7种化合物的加标回收率在68.9%~94.5%之间,日内变异系数在0.7%~3.4%之间,日间变异系数在1.5%~4.8%之间。本研究实现了牛奶中3种广谱驱虫类药物及其4种代谢物的准确定量分析,方法检出限低,回收率高,稳定性良好,填补了测定牛奶中广谱驱虫类药物液相色谱方法的空白。
This study established a high performance liquid chromatography quantitative analysis method that can simultaneously determine the residual amounts of albendazole,flubendazole,thiabendazole and four metabolites in milk.The sample was extracted with 10 mL of acetonitrile,5 mL of the extract was dried with nitrogen,dissolved in 10%hydrochloric acid solution,purified with a C18 solid phase extraction column,the purified solution was injected into the high performance liquid chromatograph,and separated by a C18 reversed-phase chromatographic column.Measured at a wavelength of 292nm,and quantified by external standard method.The results show that the 7 compounds have a good linear relationship in the range of 0.05~100μg/mL,and the correlation coefficients are all≥0.9998;the detection limit of thiabendazole is 0.025mg/kg,the limit of quantification is 0.10mg/kg,the detection limit of other 6 compounds is 0.05mg/kg,and the limit of quantification is 0.20mg/kg;the spiked recoveries of the 7 compounds are between 68.9%~94.5%,and the intra-day coefficient of variation is between 0.7%~3.4%.The day-to-day coefficient of variation is between 1.5%~4.8%.This study has achieved accurate quantitative analysis of 3 broad-spectrum anthelmintic drugs and 4 metabolites in milk.The method has low detection limit,high recovery rate and good stability,which can fill the determination of broadspectrum anthelmintic drugs in milk.It fills the gap in the liquid chromatography method for the determination of broadspectrum anthelmintic drugs in milk.
作者
赵雪宁
雷浩
贺习文
高勤叶
李易轩
ZHAO Xue-ning;LEI Hao;HE Xi-wen;GAO Qin-ye;LI Yi-xuan(Shaanxi Qin Yun Agricultural Products Inspection and Testing Co.,Ltd,Weinan 714000)
出处
《中国奶牛》
2022年第7期49-52,共4页
China Dairy Cattle
关键词
高效液相色谱法
阿苯达唑
噻苯达唑
氟苯达唑
固相萃取技术
High performance liquid chromatography
Albendazole
Thiabendazole
Flubendazole
Solid phase extraction technology
