固相萃取-高效液相色谱法测定肉制品中8种人工合成色素

Determination of 8 synthetic pigments in meat product by solid phase extraction-high performance liquid chromatography

目的建立肉制品中柠檬黄、苋菜红、胭脂红、日落黄、诱惑红、红2G、亮蓝、赤藓红的固相萃取-高效液相色谱方法。方法样品用3%氨水-甲醇提取,正己烷脱脂,过PWAX固相萃取柱净化,用2 ml 50%甲醇-水溶解样品,高速离心后,进行高效液相色谱分析;采用甲醇-0.02 mol/L乙酸铵为流动相,梯度洗脱分离,利用每种人工合成色素最大吸收波长,在检测过程中采用4种可见光波长,避免杂质干扰。结果 8种合成色素的质量浓度为0.5 mg/L^10.0 mg/L时,其峰面积与质量浓度呈良好的线性关系,相关系数(r)为0.999 5~0.999 9;检出限为0.07 mg/kg^0.23 mg/kg,回收率为80.0%~98.0%,相对标准偏差(RSD)为1.8%~5.6%。结论该方法净化效果好,回收率稳定,一次处理,可进行8种人工合成色素的测定,提高工作效率,可应用于肉制品等基质复杂样品中人工合成色素的测定。

Objective To establish a method for the determination of tartrazine,amaranth,carmine,sunset yellow,allura red,red 2G,brilliant blue,etythrosine in meat product by solid phase extraction- high performance liquid chromatography. Methods The sample was extracted with 3% ammonia water- methanol,the extract was defatted with n- hexane. After that the extract was purified with a PWAX solid phase extraction cartridge. The samples were dissolved in 50% methanol- water and the supernatant was directly injected into HPLC after high speed centrifugation. The HPLC separation was utilizing a gradient elution program of methanol and 0. 02 mol / L ammonium acetate as the mobile phase. The most absorption wavelength of every synthetic pigment was used in this process. And by adopting 4 visible lights,there was no interferences from impurities. Results When the concentration of 8 kinds of synthetic pigment was among 0. 5 mg / L- 10. 0 mg / L,the peak area and mass concentration showed a good linear relationship. The correlation coefficients（ r） of the method were among 0. 999 5- 0. 999 9; The detection limit was among 0. 07 mg / kg- 0. 23 mg / kg. The average recoveries were among 80. 0%- 98. 0%,with the RSDs among 1. 8%-5. 6%. Conclusion This method has good purification effect and stable recoveries,8 kinds of synthetic pigments can be carried out in one time treatment,work efficiency was improved,and it can be used for the determination of 8 stythetic pigments in meat products.