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

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

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 m)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。

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 m) 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.