摘要
建立了同时快速测定禽蛋中16种咪唑类药物及其代谢物的超高效合相色谱(UPC2)方法。样品用乙腈提取,经PRIME HLB柱净化,采用ACQUITY UPC2HSS C18SB色谱柱分离;以超临界二氧化碳为主要流动相,甲醇为改性剂,在35℃、12.41 MPa条件下梯度洗脱;二极管阵列检测器(PDA)检测,外标法定量。结果表明,16种咪唑类药物及其代谢物在0.2~20 mg/L浓度范围内(三氯苯达唑(TCDZ)和奥芬达唑(OFDZ)在0.4~20 mg/L范围)线性关系良好,线性相关系数均不低于0.998,检出限(LODs)为1.5~3.0μg/kg,定量限(LOQs)为5.0~10.0μg/kg。在高(250μg/kg)、中(100μg/kg)、低(5μg/kg或10μg/kg)3个浓度水平下进行加标实验,16种目标物质的加标回收率为80.9%118.4%,相对标准偏差为0.5%4.7%。该方法适用于禽蛋中咪唑类药物及其代谢物的快速分析。
An ultra-high performance convergence chromatography(UPC2)method was developed for the simultaneous determination of 16 imidazole drugs and their metabolites in poultry eggs.The samples were extracted with acetonitrile,purified by the PRIME HLB column,and separated by the ACQUITY UPC°HSS Cis SB column.With supercritical carbon dioxide as the main mobile phase and methanol as the modifier,gradient elution was performed at 35 C and 12.41 MPa.The 16 imidazole drugs and their metabolites were detected by a diode array detector(PDA)and quantitated by an external standard method.The results showed that the 16 imidazole drugs and their metabolites had good linear linearities in the concentration ranges of 0.2-20 mg/L(except trichlorobenzothiazole(TCDZ)and orfendazole(OFDZ)in the concentration ranges of O.4-20 mg/L),and the linear correlation coefficients were not less than 0.998.The limits of detection(LODs)were 1.5-3.0μg/kg,and the limits of quantification(LOQs)were 5.0-10.0μg/kg.The recoveries of 16 target substances ranged from 80.9%to 118.4%and the relative standard deviations were 0.5%-4.7%at three concentration levels of high(250μg/kg),medium(100μg/kg),and low(5μg/kg or 10μg/kg).The method is suitable for rapid analysis of imidazoles and their metabolites in poultry eggs.
作者
邱月
谭超兰
陆嘉莉
龚迎昆
余秋玲
QIU Yue;TAN Chaolan;LU Jiali;GONG Yingkun;YU Qiulingg(Chongqing Academy of Metrology and Quality Inspection,Chongqing 401123,China)
出处
《分析试验室》
北大核心
2025年第6期894-899,共6页
Chinese Journal of Analysis Laboratory
基金
重庆市科技局科研院所绩效激励引导专项(cstc2022jxjl50001)
国家市场监督管理总局科技计划项目(2023MK106)
重庆市市场监督管理局科研计划项目(CQSJKJ2022040,CQSJKJDW2023003)资助。
关键词
超高效合相色谱法
禽蛋
咪唑类药物
代谢物
ultra-high performance convergence chromatography(UPC°)
poultry eggs
imidazole drugs
metabolite
