固相萃取-超高效液相色谱法测定肉及肉制品中8种水溶性染料

Determination of 8 water-soluble dyes in meat and meat productsby solid phase extraction-ultrahigh performance liquid chromatography

目的建立固相萃取-超高效液相色谱法同时测定肉及肉制品中8种水溶性染料(喹啉黄、酸性橙12、碱性橙21、碱性橙22、酸性红2G、偶氮玉红、亮黑、荧光桃红)。方法样品经20%甲醇超声提取,过WAX固相萃取小柱净化富集,C18色谱柱分离,以甲醇-乙酸铵溶液为流动相梯度洗脱,采用液相色谱二极管阵列检测器测定,外标法定量。结果在优化后的测定条件下,8种水溶性染料在0.050~50.0 mg/L质量浓度范围内线性良好,相关系数(r)≥0.9990。方法检出限为0.008~0.06 mg/kg,回收率为81.1%~108.4%,相对标准偏差(relative standard deviation,RSD)为1.8%~6.1%。将建立的方法用于采集的23个肉及肉制品样品中,1个香肠样品检出酸性红2G,1个鱼肉样品中检出碱性橙21,含量分别为2.48 mg/kg和2.09 mg/kg。结论建立的方法准确、灵敏,适用于肉及肉制品中8种水溶性染料的同时测定。

Objective To establish a method for simultaneous determination of 8 water-soluble dyes including quinoline yellow,acid orange 12,basic orange 21,basic orange 22,acid red 2G,azorubin,bright black,and fluorescent pink in meat and meat products by solid phase extraction combined with ultrahigh performance liquid chromatography.Methods The samples were extracted with a simple ultrasonic extraction procedure with 20%methanol and cleaned up on a C18 cartridge.The analyte was separated by C18 column with the mobile phase consisting of methanol-ammonium acetate solution under gradient elution mode and detected by diode array detector.Results Under the optimized detection conditions,a good linear relationship was achieved as the mass concentrations of the 8 water-soluble dyes ranged from 0.050 mg/L to 50.0 mg/L,and the correlation coefficient(r)was≥0.9990.The method detection limits were between 0.008 mg/kg and 0.06 mg/kg.Satisfactory recoveries were obtained with the values of 81.1%-108.4%,and the relative standard deviations(RSDs)were 1.8%-6.1%.The method developed was applied to the determination of the 8 water-soluble dyes in 23 samples of meat and meat products.Acid red 2G was detected in one sample of sausage,and alkaline orange 21 was found in one sample of fish,with the values being 2.48 mg/kg and 2.09 mg/kg,respectively.Conclusion The method developed is sensitive and accurate,and it is suitable for simultaneous determination of the 8 water-soluble dyes in meat and meat products.