超高效液相色谱-串联质谱法测定水产品中的硝基呋喃代谢物
王跃,尹燕杰,赵丹,董海天,王鹏,田丽月
哈尔滨市食品药品检验检测中心,哈尔滨 150001
Determination of nitrofuran metabolites in aquatic product by UPLC-MS/MS
王跃,尹燕杰,赵丹,董海天,王鹏,田丽月
Harbin Food and Drug Inspection and Testing Center, Harbin 150001, China
摘要:建立超高效液相色谱-串联质谱法同时测定水产品中的呋喃唑酮、呋喃它酮、呋喃妥因和呋喃西林4种硝基呋喃代谢物的方法。样品经甲醇、乙醇、乙醚洗涤除杂后,进行衍生,再用Oasis HLB型固相萃取柱净化,在正离子模式下,采用MRM模式同时测定水产品中的呋喃唑酮、呋喃它酮、呋喃妥因和呋喃西林。在优化后的仪器工作条件下进行测定,4种代谢物的质量浓度在0.1~10 ng/mL的范围内线性关系良好,相关系数在0.9996~0.9999之间,检出限均为0.05 μg/kg。测定结果的相对标准偏差为1.5%~4.2%(n=5),加标回收率为87.3%~94.5%。该方法具有良好的精密度与准确度,可用于同时测定水产品中的呋喃唑酮、呋喃它酮、呋喃妥因和呋喃西林4种硝基呋喃代谢物。
Abstract:A method for the determination of the four metabolites furazolidone, furaltadone, furantoin and furacilin in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed. Samples were washed by methanol, ethanol and ether for derivatization and purified by Oasis HLB solid phase extraction column, and then detected in MRM mode via positive electrospray ionization(ESI+). After optimization of instrument operating conditions, four kind of nitrofuran metabolites had good linear relationship in the range of 0.1-10 ng/mL, the correlation coefficients were 0.9996-0.9999, the detection limits were all 0.05 μg/kg. The relative standard deviations of determination results were 1.5%-4.2%(n=5), and the average recovery rates were 87.3%-94.5%. The method has good precision and accuracy, and it is suitable for the determination of four metabolites furazolidone, furaltadone, furantoin and furacilin in aquatic products at the same time.
关键词:超高效液相色谱-串联质谱法;水产品;呋喃唑酮;呋喃它酮;呋喃妥因;呋喃西林
Keywords:ultra performance liquid chromatography-tandem mass spectrometry; aquatic product; furazolidone; furaltadone; furantoin; furacilin
本文引用格式:
王跃,尹燕杰,赵丹,等.超高效液相色谱-串联质谱法测定水产品中的硝基呋喃代谢物[J].化学分析计量,2018,27(5):43-47.
WANG Y,YIN Y J,ZHAO D,et al. Determination of nitrofuran metabolites in aquatic product by UPLC-MS/MS[J]. Chemical analysis and meterage,2018,27(5):43-47.
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