提出了液相色谱-串联质谱法测定虾肉中7种非食用色素的残留量。样品经过乙腈提取、正己烷脱脂、无水硫酸钠干燥和硅胶固相萃取柱净化。以Agilent Eclipse XDB-C8色谱柱为分离柱,采用电喷雾离子源多反应监测模式检测。采用同位素内标法定量。酸性橙2、颜料红53和酸性金黄G的线性范围在100 μg·L-1以内,其余4种色素的线性范围在10 μg·L-1以内。酸性橙2、颜料红53和酸性金黄G的测定下限(10S/N)为5 μg·kg-1,其余4种色素的测定下限(10S/N)为0.5 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率在53.8%~106%之间,测定值的相对标准偏差(n=6)在2.1%~11%之间。

A method of LC-MS/MS for the determination of residual amounts of 7 non-edible pigments in shrimp meat was proposed. The sample was extracted with acetonitrile,defatted by n-hexane,dried by anhydrous sodium sulfate,and cleaned up with SPE column filled with silica gel. Agilent Eclipse XDB-C8 chromatographic column was used as stationary phase. ESI and multi-reaction monitoring were adopted in MS/MS. Isotope was used as internal standard. Linearity ranges of acid orange 2,pigment red 53 and metanil yellow G were found in the range within 100 μg·L-1 and of the remainder 4 pigments were in the range within 10 μg·L-1. Values of lower limits of determination (10S/N) of 5 μg·kg-1 for acid orange 2,pigment red 53 and metanil yellow G and of 0.5 μg·kg-1 for the remainder 4 pigments. On the base of blank sample,test for recovery was made by standard addition method; values of recovery found were in the range of 53.8%-106%,with RSD′s (n=6) in the range of 2.1%-11%.