食品虾仁中土霉素、四环素、金霉素含量测定方法的建立

Establishment of the Method to Determine Terramycin,Tetracycline and Chlorotetracycline in Shrimp Meat

目的:建立高效液相色谱法测定虾仁中土霉素、四环素、金霉素的含量。方法:采用C18色谱柱(250 mm×4.6 mm,5μm);梯度洗脱,以甲醇为流动相A,乙腈为流动相B,10 mmol·L-1三氟乙酸为流动相C;流速1.5 m L·min-1;检测波长为350 nm。结果:土霉素、四环素、金霉素检出限分别为0.005、0.005和0.020 mg·kg-1,土霉素、四环素线性范围为0.05~1.00μg·m L-1,相关系数为0.9996及0.9995,金霉素线性范围为0.20~4.00μg·m L-1,相关系数为0.9998;加标回收率为73.5%~94.2%。结论:本方法简便、灵敏、专属,重复性好,可用于同时测定虾仁中土霉素、四环素、金霉素的含量。

Objective To establish an HPLC method to determine Terramycin, Tetracycline andChlorotetracycline in shrimp meat. Methods： The column was C18 （250 mmx4.6 mm, 5μm）. The gradientelution program was used with a flow rate of 1.5 μg · mL-1 and UV detection at 350 nm. Mobile phase Awas methyl alcohol; mobile phase B was acetonitrile; mobile phase C was 10 mmol · L-1 trifluoroaceticacid. Results： The detection limit of Terramycin, Tetracycline and Chlorotetracycline was 0.005 mg · kg-1,0.005 mg · kg-1 and 0.020 mg· kg-1, respectively. The linear range of Terramycin and Tetracycline was0.05-1.00 μg · mL-1. The correlation coefficients were 0.9996 and 0.9995, respectively. The linear range ofChlorotetracycline was 0.20-4.00 μg · mL-1, The correlation coefficient was 0.9998. The recovery rate was73.5%-94.2%. Conclusion： This method was simple, sensitive, exclusive and reproducible, which couldbe used for simultaneous determination of Terramycin, Tetracycline and Chlorotetracycline in dried shrimpmeat.