液相色谱串联质谱法测定氨糖软骨素片中硝基呋喃类代谢物残留

Determination of nitrofuran metabolites residues in glucosamine chondroitin tablets by liquid chromatography tandem mass spectrometry

中文关键词:  氨糖软骨素  硝基呋喃类代谢物  液相色谱-串联质谱法

英文关键词:glucosamine chondroitin  nitrofuran metabolites  liquid chromatography tandem mass spectrometry

中文摘要:

      目的 采用液相色谱串联质谱法测定氨糖软骨素片中的硝基呋喃类代谢物残留量。方法 样品在酸性条件下(pH<2)衍生16 h, 经乙酸乙酯提取浓缩。经甲醇水溶液溶解过滤后, 用液相色谱-串联质谱测定。试验过程中采用添加同位素内标法来补偿前处理过程中产生的损失。结果 在0.5、1.0和2.0 μg/kg 3个浓度水平上进行添加回收试验, 4种代谢物的回收率范围为82.7~106.7%, 相对标准偏差不大于12.3%, 检出限均为0.5 μg/kg。结论 该方法具有良好的准确度、灵敏度和稳定性, 可用于氨糖软骨素片中硝基呋喃类代谢物残留量的测定。

英文摘要:

      Objective To determine the residue of nitrofuran metabolites inglucosamine chondroitin tablets by liquid chromatography tandem mass spectrometry. Methods The sample was derived 16 h in acid condition (pH<2), and then extracted and concentrated by ethyl acetate. The extract was dissolved and filtered by methanol-water and determined by liquid chromatography tandem mass spectrometry. The isotope internal standard method was used in the experiment to compensate the loss in the pretreatment. Results The recovery experiments were conducted at levels of 0.5, 1.0 and 2.0 μg/kg, and the recoveries of the four metabolites ranged in 82.7%-106.7% with RSD≤12.3%. The limit of detection was 0.5 μg/kg. Conclusion The method has good accuracy, sensitivity and stability and can be used for the determination of residual nitrofuran metabolites in glucosamine chondroitin tablets.