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建立了一种以牛肉中肌肽为代表,反相分离测定亲水性物质的方法。选用丙基酰胺键合硅胶亲水作用色谱柱,反相分析测定牛肉中亲水性成分-肌肽的含量,样品无需衍生处理。结合HPLC-MS联用技术确定了保留时间为10.276~10.609 min的色谱峰就是肌肽峰。将该色谱柱与常规C18色谱柱进行对比后发现,该色谱柱对L-肌肽的保留能力和分离能力均优于C18柱,RSD%为1.1%,检测限为4.59×10-2mg/L。实验结果表明:亲水性色谱柱反相使用时,完全适用强极性物质含量的测定,方法已用于牛肉中肌肽含量的测定。
A method for the determination of hydrophilic material by reversed-phase method was established, which is represented by carnosine in muscle. Propyl amide bonded silica hydrophilic column was used to determine the content of carnosine, the hydrophilic component of beef, by reversed-phase analysis. No derivatization was required for the samples. Combined with HPLC-MS technology to determine the retention time of 10.276 ~ 10.609 min chromatographic peak is the carnosine peak. Compared with the conventional C18 column, the column has better retention and separation ability than C18 column with RSD% of 1.1% and detection limit of 4.59 × 10-2 mg / L. The experimental results show that when the hydrophilic column is reversed-phase, the determination of strongly polar substances is fully applicable. The method has been applied to the determination of carnosine in beef.