超高效液相色谱-串联四级杆质谱测定肝素中硝基呋喃代谢物残留

 目的 建立超高效液相色谱-串联四级杆质谱测定动物源性药物肝素中4种硝基呋喃代谢物残留的方法。方法 样品在酸性条件下水解,经2-硝基苯甲醛(2 - NBA) 37 ℃衍生化16 h,乙酸乙酯提取后,采用电喷雾电离,正离子扫描,多反应监测模式（MRM）检测,内标法定量测定。结果 硝基呋喃代谢物线性范围分别在0.1～10.0 μg·L^-1之间;r分别在0.994～0.996之间;检出浓度分别在0.08～0.226 μg·kg^-1之间;回收率分别在82.4%～109.7%之间。结论 该方法快速、准确、灵敏,可作为肝素中4种硝基呋喃代谢物的测定。

Determination of Four Nitrofuran Metabolites in Heparin by UPLC-MS/MS

Objective To establish a method for determination of four nitrofuran metabolites in animal-derived heparin by UPLC triple-quadruple tandem mass spectrometer. METHODS Samples are hydrolyzed with hydrochloric acid,and derivatized at 37 ℃ for 16 h with 2-nitrobenzaldehyde.The target compounds are eluted with ethyl acetate. Identification is achieved by electrospray ionization in positive mode(ESI⁺) using multiple reaction monitoring(MRM). The quantification is performed with internal standards. RESULTS A linearity of nitrofuran antibiotics is obtained from 0.1 to 10.0μg·L^-1. r are 0.994-0.996. The LODs are between 0.08-0.226 μg·kg^-1and the average recoveries are 82.4%-109.7% respectively. CONCLUSION The method is rapid,precise,sensitive,and suitable for the determination of four nitrofuran metabolites in heparin.