固相萃取-高效液相色谱同时测定干辣椒中4种橙黄染料  

Simultaneous determination of four orange dyes in dry chili by SPE-HPLC

作　　者：徐明敏[1] 陈晓红[2,3] 

机构地区：[1]宁波市北仑区疾病预防控制中心,浙江宁波315800 [2]宁波市疾病预防控制中心浙江省微量有毒化学物健康风险评估技术研究重点实验室,浙江宁波315010 [3]宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室,浙江宁波315010

出　　处：《中国卫生检验杂志》2015年第8期1115-1118,共4页Chinese Journal of Health Laboratory Technology

基　　金：浙江省自然科学基金项目(LY13B050003);浙江省医药卫生科研项目(2013KYA187);宁波市自然科学基金项目(2013A610243);宁波市农业与社会发展重点择优委托项目(2011C11021)

摘　　要：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 method for the determination of four illegal added orange dyes （ orange I , orange Ⅱ, or- ange Ⅳ and orange G） in dry chili by using solid -phase extraction （SPE） and high performance liquid chromatography （HPLC）. Methods After crushing, chili samples were extracted by methanol, purified with a WAX solid - phase extraction （SPE） cartridge, and washed by the solution of formic acid - methanol （5 ： 95, V/V） and methanol in succession, as well as eluted and quantified by ammonia- methanol （10 ： 90, V/V）. After the elution, it was dried by nitrogen and dissolved in the initial mobile phase, the separation was performed on a Zorbax SB -C_18 column （150 mm× 2.1 mm, 5 μm） with the mobile phase of methanol and 20 mmol/L ammonium acetate with a gradient elution. Detection was carried out at 470 nm, and quanti- fied with external standard. Results There were good linearity in the range of 0.5 mg,/L - 50.0 mg/L with a correlation coeffi- cient of more than 0.999 1, and the limits of quantity（LOQs） were between 0.05 mg/kg - 0.1 mg/kg. The extraction recover- ies were of 91.2% - 106.7%, and the RSD was among 1.6% - 7.7%. Conclusion The developed method is simple, fast, of little interference and good specificity for the satisfactory determination of four illegal added orange dyes （ orange I , orange Ⅱ , orange Ⅳ and orange G） in dry chili.

关 键 词：辣椒 橙黄染料 高效液相色谱法 固相萃取 

分 类 号：O657.72[理学—分析化学]