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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 To detect the metabolites of gelatin and four kinds of nitrofurans (furazolidone, furidone, nitrofurazone and nitrofurantoin) remaining in the process of production by high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS). Methods The pretreatment method was optimized to solve the problem of gel formation during sample processing. The sensitivity of detection was improved by high resolution mass spectrometry, and the internal standard method was used for the quantification. Results The linear range of the four nitrofuran metabolites was 0.5-10 μg · kg -1 with the correlation coefficients greater than 0.995 (n = 5) and the detection limit of 0.5 μg · kg -1 Rates ranged from 83.9% to 100.8% with RSDs ranging from 7.0% to 9.5%. Conclusion The method is simple, sensitive and accurate in pretreatment. It is suitable for the determination of nitrofuran metabolites in gelatin and its intermediates.