明胶及其中间体中硝基呋喃类代谢物测定方法的研究Study on the Detection of Nitrofuran Metabolites in Gelatin and Its Intermediates
林生文,靳贵英,郑传奇
LIN Shengwen,JIN Guiying,ZHENG Chuanqi
摘要(Abstract):
目的利用高效液相色谱-串联质谱法(LC-MS/MS)检测明胶及其生产过程中残留的4种硝基呋喃类药物(呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因)的代谢物。方法优化前处理方法,解决样品处理过程中结冻成胶的问题,采用高分辨质谱联用技术提高检测的灵敏度,同位素内标法定量。结果 4种硝基呋喃类代谢物线性范围为0.5~10μg·kg~(-1),相关系数均大于0.995(n=5),检出限为0.5μg·kg~(-1),平均回收率为83.9%~100.8%,RSD为7.0%~9.5%。结论该方法前处理简单,灵敏度和准确度高,适用于明胶及其生产过程中的中间体硝基呋喃类代谢物残留的检测。
OBJECTIVE The nitrofuran metabolites( AMOZ,SEM,AHD and AOZ) are determined by liquid chromatography tandem mass spec-trometry( LC-MS/MS) in gelatin products. METHODS The pretreatment method was optimized to solve the problem of gel formation during the sample preprocess. The sensitivity of detection was greatly improved by using high resolution mass spectrometry,and the isotope internal standard method was used to quantify the nitrofuran metabolites. RESULTS The linear range of4 metabolites was 0. 5-10 μg·kg~(-1),and the correlation coefficients were greater than 0. 995( n = 5). The detection limit was0.5 μg·kg~(-1),the recovery rate was 83.9%-100.8%,and RSD was 7.0%-9.5%. CONCLUSION This method is simple,sensitive and accurate. It is suitable for the detection of metabolites residues in the process of gelatin and its intermediates.
关键词(KeyWords):
明胶;硝基呋喃代谢物;液质联用
gelatin;nitrofuran metabolite;liquid chromatography-mass spectrometry
基金项目(Foundation): 广东省省级科技计划项目(2014A040401047)
作者(Author):
林生文,靳贵英,郑传奇
LIN Shengwen,JIN Guiying,ZHENG Chuanqi
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