固相萃取联合超高效液相色谱-串联质谱法测定畜肉中3 种儿茶酚胺类物质

建立超高效液相色谱-串联质谱技术同时检测畜肉中3 种儿茶酚胺类物质。畜肉样品用高氯酸溶液提取，经混合阳离子固相萃取小柱净化，HILIC Plus色谱柱（4.6 mm×100 mm，3.5 μm）分离，流动相分别为甲酸-水（1∶99，V/V）和乙腈，采用电喷雾离子源，正离子多反应监测，对儿茶酚胺类药物进行检测，外标法实现定量分析。结果表明：3 种儿茶酚胺类药物在40～1 000 ng/mL范围内线性良好，相关系数大于0.99，畜肉中检出限（RSN≥3）为10 μg/kg，定量限（RSN≥10）为40 μg/kg；添加量为40～1 000 μg/kg的3 种儿茶酚胺类物质的回收率均在75.48%～91.25%之间，方法的精密度在1.2%～4.6%之间（n=6）。该方法前处理简单、快速、准确，为畜肉中儿茶酚胺的检测提供方法。

Determination of Three Catecholamines in Livestock Meat by Solid Phase Extraction Combined with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

This study aimed to establish a method for simultaneous qualitative and quantitative analysis of three catecholamines (CAs) in livestock meat by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were homogenized, extracted with perchloric acid solution, and purified on a PCX solid phase extraction cartridge. The chromatographic separation was achieved on an HILIC Plus column (4.6 mm × 100 mm, 3.5 μm) using a mobile phase consisting of acetonitrile and formic acid in water (1:99, V/V). The analytes were ionized by positive electrospray (ESI+), detected in the multiple reaction monitoring mode (MRM) and quantified by the external standard method. The results indicated that a good linearity over the concentration range of 40–1 000 ng/mL was observed for all the analytes with correlation coefficients greater than 0.99. The limits of detection (LOD) and quantification (LOQ) were 10 and 40 μg/kg, respectively. The average recoveries of the CAs ranged from 75.48% to 91.25% with relative standard deviations (RSDs) of 1.2%–4.6% (n = 6). The method is sensitive, simple, rapid and accurate and can meet the requirements for practical analysis.