高效液相荧光法测定猪肉中抗氧化剂乙氧基喹啉以及代谢产物二聚乙氧基喹啉

Determination of EQ and EQDM in pork by HPLC with fluorescence detector

建立同时检测猪肉中乙氧基喹啉以及代谢产物二聚乙氧基喹啉的高效液相荧光法。方法:猪肉经匀浆机破碎后,以正己烷作为提取溶剂,按固液比1∶3(g∶mL)室温下超声提取,提取液经真空干燥后,以乙腈定容,并在C_(18)色谱柱,柱温为30℃;荧光检测器激发波长:360 nm,吸收波长:440 nm;流动相为V(乙腈)∶V(2%乙酸)=85∶15,流速:1.0 mL/min的条件下,通过高效液相荧光法检测样品中乙氧基喹啉以及二聚乙氧基喹啉的含量。结果:在该样品预处理和色谱条件下,乙氧基喹啉保留时间为5.861 min,线性回归方程为:Y=604.27X-8 446,R^2=0.993 6;二聚乙氧基喹啉保留时间为32.436 min,线性回归方程为:Y=1 425.3X-6 140.8,R^2=0.995 6,对乙氧基喹啉的回收率为93.88%~107.18%,二聚乙氧基喹啉回收率为80.74%~83.62%,RSD均小于5.00%。结论:该方法简单快速,灵敏度高,可用于猪肉中抗氧化剂乙氧基喹啉和二聚乙氧基喹啉含量的检测。

To establish a method for determination ethoxyquin and ethoxyquin dimer in pork by HPLC-FLD. After homogenized,pork was extracted by n-hexane at ratio of 5 ∶ 15（ g∶ mL） with ultrasound assistant at room temperature. The extract was dried by vacuum and fixed with acetonitrile. The content of ethoxyquin and thoxyquindimer in the sample was detected by high performance liquid chromatography with C18 chromatographic column; the column temperature was 30 ℃. Fluorescence detector was used and the excitation wavelength was 360 nm,absorption wavelength was 440 nm. Mobile phase of acetonitrile was 2% acetic acid（ 85∶ 15,V/V） at 1. 0 mL/min flow rate. Under the above conditions,the retention time of ethoxyquin was 5. 816 min,and the linear regression equation was： Y =604. 27 X-8 446,R^2= 0. 993 6. The retention time of ethoxyquin dimer was 32. 436 min,and the linear regression equation was Y = 1 425. 3 X-6 140. 8,R^2= 0. 995 6. The recovery rate of ethoxyquin was between 93. 88%-107. 18%,and the recovery rate of ethoxyquin dimer was between 80. 74%-83. 62%. The RSD is less than 5. 00%. This method is simple and rapid,high sensitivity. It can be used for detecting ethoxyquin and ethoxyquin dimer in pork.