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目的建立干辣椒中橙黄Ⅰ、橙黄Ⅱ、橙黄Ⅳ和橙黄G等4种非法添加橙黄染料的固相萃取-高效液相色谱检测方法。方法干辣椒样品经粉碎后用甲醇进行提取,用WAX固相萃取小柱进行净化,分别采用甲酸-甲醇(5:95,V/V)溶液和甲醇进行淋洗,采用氨水-甲醇(10:90,V/V)溶液进行洗脱,洗脱液经氮吹后定容,在Zorbax SB-C_(18)柱(150 mm×2.1 mm,5μm)上以甲醇-20 mmol/L乙酸铵溶液为流动相进行梯度洗脱分离,在470 nm波长处进行检测,外标法定量。结果 4种橙黄染料在0.5 mg/L~50.0 mg/L时均具有良好的线性,相关系数>0.999 1,最低定量检出限为0.05 mg/kg~0.1 mg/kg,回收率为91.2%~106.7%,RSD为1.6%~7.7%。结论建立的方法具有简便、快速、干扰少和特异性强的特点,适用于干辣椒中4种橙黄染料(橙黄Ⅰ、橙黄Ⅱ、橙黄Ⅳ和橙黄G)的非法添加检测。
OBJECTIVE To establish a solid phase extraction and high performance liquid chromatography (HPLC) method for the detection of four kinds of illegally added orange yellow dyes in orange yellow I, orange yellow II, orange yellow IV and yellow orange G, respectively. Methods The samples of dried chilli peppers were crushed and extracted with methanol. The samples were purified by WAX solid phase extraction cartridges. The samples were eluted with formic acid - methanol (5:95, V / V) and methanol, respectively, 90, V / V). The eluate was denitrified with nitrogen and diluted to volume on a Zorbax SB-C 18 column (150 mm × 2.1 mm, 5 μm) The mobile phase was eluted by gradient elution, detected at 470 nm and quantified by external standard method. Results The results showed that all four kinds of yellow orange dyes had good linearity at the concentration range of 0.5 mg / L ~ 50.0 mg / L, the correlation coefficient was> 0.999 1, the detection limit was 0.05 mg / kg ~ 0.1 mg / kg, the recovery was 91.2% 106.7%, RSD 1.6% ~ 7.7%. Conclusion The established method has the characteristics of simple, rapid, less interference and high specificity. It is suitable for the illegal addition detection of four orange yellow dyes (orange Ⅰ, yellow Ⅱ, orange Ⅳ and yellow G) in dried pepper.