固相萃取-超高效液相色谱-串联质谱法快速测定鸡粪中37种抗菌药物的含量  

Rapid Determination of 37 Antibiotics Content in Chicken Manure by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid-phase Extraction

作　　者：金晓峰 赵贵 田兵 苏伟[3] 栾庆祥 黄鑫 王璇[4] 陈灵 章厉劼 孙播东 周泽晓 王庆红 杨强 廖欢 古海 谢丽丽 母应春[3] 文正常[4] JIN Xiaofeng;ZHAO Gui;TIAN Bing;SU Wei;LUAN Qingxiang;HUANG Xin;WANG Xuan;CHEN Ling;ZHANG Lijie;SUN Bodong;ZHOU Zexiao;WANG Qinghong;YANG Qiang;LIAO Huan;GU Hai;XIE Lili;MU Yingchun;WEN Zhengchang(Guizhou Provincial Veterinary Drug and Feed Supervision Institute,Guiyang 550003;Guizhou Provincial Livestock and Poultry Germplasm Testing Center,Guiyang 550018;Guizhou University,Guiyang 550025;Guizhou Provincial Institute of Animal Husbandry and Veterinary Medicine,Guiyang 550005)

机构地区：[1]贵州省兽药饲料检测所,贵州贵阳550003 [2]贵州省种畜禽种质测定中心,贵州贵阳553018 [3]贵州大学,贵州贵阳550025 [4]贵州省畜牧兽医研究所,贵州贵阳550005

出　　处：《分析科学学报》2024年第3期315-322,共8页Journal of Analytical Science

基　　金：贵州省生态家禽产业技术体系项目(GZSTJQCYJSTX-05)。

摘　　要：建立了固相萃取-超高效液相色谱-串联质谱法(SPE-UPLC-MS/MS)快速测定鸡粪中37种抗菌药物含量的方法。鸡粪经冻干制备,80%乙腈(含0.1%甲酸)提取,Oasis PRiME HLB通过式固相萃取净化后,利用UPLC-MS/MS测定抗菌药物含量。结果表明,37种抗菌药物浓度在0.40~200.0ng/mL范围内线性关系良好,相关系数(R^(2))大于0.996,检出限(LOD)为1μg/kg,定量限(LOQ)为4μg/kg。37种抗菌药物在3个浓度添加标水平(LOQ、5倍LOQ、10倍LOQ)下的回收率为63.5%~104.2%,批内相对标准偏差为1.47%~10.5%,批间相对标准偏差为2.39%~14.2%。所建立方法准确、快速、灵敏、稳定,可实现鸡粪中37种抗菌药物的同时快速测定。A method for the rapid determination of 37 antibiotics content in chicken manure by ultra performance liquid chromatography-tandem mass spectrometry with solid-phase extraction has been developed.Chicken manure was prepared by freeze-drying and extracted with 80%acetonitrile(containing 0.1%formic acid),purified by Oasis PRiME HLB solid phase extraction and determined by UPLC-MS/MS.The results showed that there was a good linear relationship for the concentration of 37 antibiotics in the range of 0.40-200.0 ng/mL(R^(2)≥0.996).Meanwhile,the LOD and LOQ were 1μg/kg and 4μg/kg;the recovery of 37 antibiotics ranged from 63.5%to 104.2%in three concentration levels(LOQ,5 times of LOQ,10 times of LOQ).The intra-day RSD was 1.47%-10.5%,and the inter-day RSD was 2.39%-14.2%.This method is accurate,rapid,sensitive and stable.Simultaneous and rapid determination of 37 antibiotics in chicken manure has been achieved.

关 键 词：鸡粪 固相萃取 超高效液相色谱-质谱/质谱 抗菌药物 

分 类 号：O657.63[理学—分析化学]