超声探针辅助酶解结合全自动固相萃取快速测定动物组织中β-受体激动剂残留  

Enzymatic Probe Sonication Coupled with Automatic Solid-Phase Extraction for Quick Determination of β-Agonists Residues in Animal Tissues

作　　者：肖志明[1] 王石[1] 索德成[1] 李阳[1] 姚婷 娄迎霞 赵新雪 张峰 樊霞[1] XIAO Zhi-Ming;WANG Shi;SUO De-Cheng;LI Yang;YAO Ting;LOU Ying-Xia;ZHAO Xin-Xue;ZHANG Feng;FAN Xia(China National Feed Quality Control Center,Institute of Quality Standard and Testing Technology for Agro-Products,Chinese Academy of Agricultural Sciences,Beijing 100081,China;Beijing Institute of Feed Control,Beijing 100107,China;Reeko Instrument Co.Ltd.,Xiamen 361000,China)

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所,国家饲料质量检验检测中心(北京),北京100081 [2]北京市饲料监察所,北京100107 [3]睿科仪器(厦门)有限公司,厦门361000

出　　处：《分析化学》2022年第6期957-963,I0001-I0017,共24页Chinese Journal of Analytical Chemistry

基　　金：“十三五”国家重点研发计划项目(No.2018YFC1602302)资助。

摘　　要：建立了猪、牛、羊肌肉和肝脏中22种β-受体激动剂残留的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品采用β-葡萄糖醛酸酶/芳基硫酸酯酶在超声探针辅助下进行快速酶解提取,酶解后在全自动固相萃取仪上净化,UPLC-MS/MS测定,采用内标法进行定量分析。结果表明,超声探针辅助酶解在120 s内即达到了传统酶解16 h的提取效率,回收率为81.2%~100.7%。结合全自动固相萃取的批量、自动化处理,30 min内可同时处理36份样品,显著提升了工作效率,避免了因人员操作导致的结果偏差,相对标准偏差低至0.3%~7.9%。与传统酶解和固相萃取方法相比,本方法具有快速、简便和高通量等优点,适用于大批量动物组织样品的日常监测。An ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method has been developed for determination of 22 kinds of β-agonists residues in swine, bovine and sheep muscle and liver samples. The animal food samples were extracted with enzymatic probe sonication(EPS)using β-glucuronidase/sulfatase enzymes, followed by clean-up using automatic solid-phase extraction and determination by UPLC-MS/MS. The target analytes were quantified by internal standard methods. Under the optimized EPS conditions, one sample could be exhaustively extracted within 120 s(average recovery 81.2% –100.7%), as compared with 16 h needed for the conventional enzymatic digestion, which was more suitable for high-throughput screening. Furthermore, the clean-up was conducted using automatic solid-phase extraction, and 36 samples could be performed in 30 min simultaneously. The work efficiency was significantly improved, and the relative standard deviations(RSDs)were relatively low(0.3%–7.9%).As compared with the traditional enzymatic digestion and solid-phase extraction techniques, the newly developed method was quick and easy to be performed, which was more suitable for high-throughput detection in routine residual analysis.

关 键 词：β-受体激动剂 超声探针辅助酶解 全自动固相萃取 动物组织 

分 类 号：O657.63[理学—分析化学] S859.84[理学—化学]