College of Biological and Chemical Engineering, Zhejiang University of Science and Technology, Hangzhou 310023, China.
College of Biotechnology and Bioengineering, Zhejiang University of Technology, Hangzhou 310014, China.
Molecules. 2023 Feb 21;28(5):2039. doi: 10.3390/molecules28052039.
β-agonists are a class of synthetic sympathomimetic drugs with acute poisoning effects if consumed as residues in foods. To improve the efficiency of sample preparation and to overcome matrix-dependent signal suppression in the quantitative analysis of four β-agonists (clenbuterol, ractopamine, salbutamol, and terbutaline) residues in fermented ham, an enzyme digestion coupled cation exchange purification method for sample preparation was established using ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS). Enzymatic digests were subject to cleanup treatment on three different solid phase extraction (SPE) columns and a polymer-based strong cation resin (SCR) cartridge containing sulfonic resin was found to be optimal compared with silica-based sulfonic acid and polymer sulfonic acid resins based SPEs. The analytes were investigated over the linear range of 0.5 to 10.0 μg/kg with recovery rates of 76.0-102.0%, and a relative standard deviation of 1.8-13.3% (n = 6). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.1 μg/kg and 0.3 μg/kg, respectively. This newly developed method was applied to the detection of β-agonist residues in 50 commercial ham products and only one sample was found to contain β-agonist residues (clenbuterol at 15.2 µg/kg).
β-激动剂是一类合成拟交感神经药物，如果作为残留物存在于食物中，会产生急性中毒效应。为了提高样品制备的效率，并克服发酵火腿中四种β-激动剂（克仑特罗、莱克多巴胺、沙丁胺醇和特布他林）残留量定量分析中的基质依赖信号抑制问题，建立了一种酶解结合阳离子交换净化的方法，用于超高效液相色谱串联质谱（UHPLC-MS/MS）分析。酶解产物经过三种不同固相萃取（SPE）柱的净化处理，与基于硅胶的磺酸 SPE 相比，含有磺酸基的聚合物强阳离子树脂（SCR）柱被发现是最佳的。在 0.5 至 10.0 μg/kg 的线性范围内对分析物进行了研究，回收率为 76.0-102.0%，相对标准偏差为 1.8-13.3%（n = 6）。检测限（LOD）和定量限（LOQ）分别为 0.1 μg/kg 和 0.3 μg/kg。该新方法应用于 50 种市售火腿产品中β-激动剂残留量的检测，仅发现一个样品含有β-激动剂残留（克仑特罗为 15.2 µg/kg）。
