液相色谱-串联质谱联用法测定干海参中硝基呋喃代谢物残留量

Determination of antibiotics nitrofuran metabolites in dried sea cucumber by HPLC-MS / MS

建立了检测干海参中4种硝基呋喃代谢物的高效液相色谱-串联质谱方法。将干海参样品经过盐酸水解,以2-硝基苯甲醛(2-NBA)为衍生剂,经HLB固相萃取净化后,用高效液相色谱-串联质谱(ESI+)MRM检测,同位素内标定量。结果表明:4种硝基呋喃代谢物的线性范围均为0.5~10.0μg/L,检出限均为0.5μg/kg,3个水平的加标回收率为76.4%~88.4%。该方法稳定性强、重现性好,能满足干海参中4种硝基呋喃代谢物残留检测的要求。

A method for detection of 4 metabolites of antibiotics nitrofuran was developed in dried sea cucumber by HPLC-MS / MS. Samples of the dried sea cucumber were hydrolyzed by hydrochloric acid and derived with 2-nitrobenzaldehyde,was purified by HLB solid-phase extraction,and analyzed by HPLC-MS / MS( ESI+) using multiple reaction monitoring( MRM) in which the quantitative analysis was carried out by isotope internal standard dilution technique. The metabolite levels of antibiotics nitrofuran were shown a good linear relationship over the concentration ranging from 0. 5 μg / L to 10. 0 μg / L,with the detection limit of 0. 5 μg / kg,and average recovery from 76. 4% to 88. 4%,indicating that the method has strong stability,good reproducibility,and meet the requirements for detection of nitrofuran metabolites in dried sea cucumber.