高效液相色谱-质谱法测定畜肉中的卡拉胶

Determination of Carrageenan in Livestock Meat by High Performance Liquid Chromatography-Mass Spectrometry

建立测定畜肉中卡拉胶的高效液相色谱-质谱法。生鲜肉样品用1 mol/L盐酸处理,其中的卡拉胶降解生成[A-G4S]-等特征性寡糖片段,采用高效液相色谱-三重四极杆质谱进行定性和定量测定。可选择高分辨质谱用于确证。结果表明,对于正常畜肉样品不出现假阳性,对于标识添加卡拉胶的调理牛排等阳性样品均能有效识别。对于m/z 403>241离子对,检出限为20 mg/kg(卡拉胶/肉),线性范围为0.1～0.4 g/kg,线性相关系数在0.99以上,相对回收率为90%～120%。该方法前处理简便、检测指标明确、灵敏度高,可作为检测添加卡拉胶畜肉的有效手段。

This study aimed to establish a method for the determination of added carrageenan in livestock meat by high performance liquid chromatography-mass spectrometry(HPLC-MS). Carrageenan in fresh meat was digested with 1 mol/L hydrochloric acid, yielding characteristic oligosaccharide fragments such as [A-G4 S]-, which were detected by HPLC-triple quadrupole mass spectrometry. A high resolution mass spectrometer was employed for validation of the method. The results showed that no false positive results were found for natural meat samples, while positive samples such as steak labelled to contain carrageenan were identified effectively by the proposed method. The limit of detection(LOD) of carrageenan was20 mg/kg(at m/z 403 > 241). A good linear relationship was observed in the concentration range of 0.1–0.4 g/kg with correlation coefflcients of more than 0.99. The relative recoveries were in the range of 90%–120%. In summary, this method, thanks to its simplicity, clear target and high sensitivity, could be used as an effective means to detect carrageenan-injected livestock meat.